CN112266253A - Granular material of microwave medium material for injection moulding and method for manufacturing microwave medium device - Google Patents
Granular material of microwave medium material for injection moulding and method for manufacturing microwave medium device Download PDFInfo
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- CN112266253A CN112266253A CN202010997552.XA CN202010997552A CN112266253A CN 112266253 A CN112266253 A CN 112266253A CN 202010997552 A CN202010997552 A CN 202010997552A CN 112266253 A CN112266253 A CN 112266253A
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000001746 injection moulding Methods 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 title claims description 54
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 239000008187 granular material Substances 0.000 title claims description 5
- 239000003989 dielectric material Substances 0.000 claims abstract description 39
- 239000011230 binding agent Substances 0.000 claims abstract description 34
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000853 adhesive Substances 0.000 claims abstract description 11
- 230000001070 adhesive effect Effects 0.000 claims abstract description 11
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004743 Polypropylene Substances 0.000 claims abstract description 7
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 7
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 7
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims abstract description 7
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 7
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 7
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 7
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 7
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 7
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 7
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 7
- -1 polypropylene Polymers 0.000 claims abstract description 7
- 229920001155 polypropylene Polymers 0.000 claims abstract description 7
- 239000008117 stearic acid Substances 0.000 claims abstract description 7
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 46
- 238000005238 degreasing Methods 0.000 claims description 42
- 238000005245 sintering Methods 0.000 claims description 26
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 230000000630 rising effect Effects 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 abstract description 11
- 239000008188 pellet Substances 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
The pellet of microwave dielectric material for injection molding and the microwave dielectric device producing process include the following steps: 70-90% of microwave dielectric material and 10-30% of binder, wherein the microwave dielectric material comprises 60-70% of titanium dioxide, 25-35% of magnesium oxide, 2-8% of calcium carbonate, 2-8% of barium carbonate, 0.1-1% of niobium pentoxide and 0.1-1% of bismuth trioxide; the adhesive comprises 70-90% of polyformaldehyde, 2-15% of polymethyl methacrylate, 2-15% of polypropylene, 2-15% of ethylene-vinyl acetate copolymer, 2-10% of wax, 1-3% of dioctyl phthalate, 1-3% of dibutyl phthalate and 1-5% of stearic acid. Relative dielectric constant of microwave dielectric device manufactured by the inventionεrQ x f value, temperature coefficient of resonance frequency taufCompared with the traditional method, the method has the advantages that the crystal grains of the sample are compact, fine and uniform.
Description
Technical Field
The invention relates to a microwave dielectric material, in particular to a pellet of the microwave dielectric material for injection molding and a method for manufacturing a microwave dielectric device.
Background
The traditional production process technology of microwave medium samples is mainly a dry pressing forming method, and the method has the defects that the shape of a formed product is greatly limited, the strength of a blank is low, the compactness of the interior of the blank is inconsistent, the uniformity of a tissue structure is relatively poor, and the like.
The above background disclosure is only for the purpose of assisting understanding of the inventive concept and technical solutions of the present invention, and does not necessarily belong to the prior art of the present patent application, and should not be used for evaluating the novelty and inventive step of the present application in the case that there is no clear evidence that the above content is disclosed at the filing date of the present patent application.
Disclosure of Invention
In order to overcome at least one of the technical defects, the invention provides a granular material of a microwave dielectric material for injection molding, a preparation method of a microwave dielectric material blank and a manufacturing method of a microwave dielectric device.
The granular material of microwave dielectric material for injection molding includes microwave dielectric material in 70-90 wt% and adhesive in 10-30 wt%; the microwave dielectric material comprises the following components in percentage by weight: 60 to 70 percent of titanium dioxide, 25 to 35 percent of magnesium oxide, 2 to 8 percent of calcium carbonate, 2 to 8 percent of barium carbonate, 0.1 to 1 percent of niobium pentoxide and 0.1 to 1 percent of bismuth trioxide; the adhesive comprises the following components in percentage by weight: 70-90% of polyformaldehyde, 2-15% of polymethyl methacrylate, 2-15% of polypropylene, 2-15% of ethylene-vinyl acetate copolymer, 2-10% of wax, 1-3% of dioctyl phthalate, 1-3% of dibutyl phthalate and 1-5% of stearic acid.
A preparation method of a microwave dielectric material blank comprises the following steps:
s1, preparing a microwave dielectric material and a binder, wherein the microwave dielectric material comprises, by weight, 70% -90% of titanium dioxide, 25% -35% of magnesium oxide, 2% -8% of calcium carbonate, 2% -8% of barium carbonate, 0.1% -1% of niobium pentoxide and 0.1% -1% of bismuth trioxide, and the binder accounts for 10% -30%; the adhesive comprises 70-90% of polyformaldehyde, 2-15% of polymethyl methacrylate, 2-15% of polypropylene, 2-15% of ethylene-vinyl acetate copolymer, 2-10% of wax, 1-3% of dioctyl phthalate, 1-3% of dibutyl phthalate and 1-5% of stearic acid;
s2, banburying and granulating the materials prepared in the step S1;
and S3, performing injection molding on the material obtained in the step S2 to obtain the microwave dielectric material blank.
Further:
in step S3, the material is heated and melted in a barrel of an injection machine at 150-200 ℃, and the melted material is injected into a die cavity under the pressure of 100-150 Bar to fill the die cavity.
In step S3, after the product and the nozzle material are separated in the mold by the in-mold nozzle cutting technique, the product is taken out of the mold.
The manufacturing method of the microwave dielectric device comprises the steps of degreasing and sintering the microwave dielectric material blank prepared by the preparation method of the microwave dielectric material blank to obtain the microwave dielectric device.
Further:
the degreasing comprises acid-catalyzed degreasing and thermal degreasing which are sequentially carried out.
The acid catalytic degreasing is performed by using nitric acid or oxalic acid at a heating rate of 0.3-1.0 ℃/min to 100-200 ℃.
The thermal degreasing is carried out under the condition that the temperature is raised to 150-450 ℃ at the temperature rise speed of 0.2-0.8 ℃/min.
The sintering comprises the following steps:
a temperature rising stage: slowly raising the temperature from room temperature to 400-500 ℃ at a temperature raising rate of 0.2-0.8 ℃/min, and after the binder is discharged, continuing raising the temperature to 850-950 ℃ at a temperature raising rate of 1.0-2.0 ℃/min;
and (3) a blank gradual shrinkage stage: continuously heating to 1300-1400 ℃ at a heating rate of 0.5-1.5 ℃/min;
and (3) a heat preservation stage: preserving the heat for 1 to 3 hours at the temperature of between 1300 and 1400 ℃;
and (3) cooling: cooling at a cooling rate of 0.5 ℃/min to 2.0 ℃/min.
The acid-catalyzed degreasing is carried out in nitrogen; the thermal degreasing and the sintering are both performed in air.
Compared with the prior art, the invention has the following beneficial effects:
the injection molding formula and the manufacturing process of the microwave dielectric device provided by the invention effectively overcome the defects of the existing dry pressing molding technology, solve the problem of molding the microwave dielectric device with a complex shape, improve the performance of the product and improve the production efficiency.
The injection molding formula material is used for banburying and granulating, simultaneously the problem of manufacturing microwave devices with complex shapes is well solved, the consistency of products is good, and the density of the products is large and uniform. Product testing found that the product has dense, fine and uniform grains as seen from the surface and internal microstructures of the product made by the present invention. The density of the microwave device obtained by the method of the invention is higher than that of the product obtained by the conventional method, and the relative dielectric constant epsilonrQ x f value, temperature coefficient of resonance frequency taufIt is also better than the conventional one.
The microwave dielectric device is produced by using the injection molding formula and the process in one step, and does not need to be pressed into a blank body firstly and then machined like the traditional dry pressing process. The process based on the injection molding formula material of the invention heats and melts the material, injects the melted material into the die cavity under high pressure, opens the die after the die cavity is filled, takes out the solidified blank, has no stress in the blank, and has one-step molding without processing. Further, by adopting the technology of cutting the nozzle in the die, the product and the nozzle material are separated in the die.
Drawings
Fig. 1 is a process flow diagram of a manufacturing method of an injection microwave dielectric device according to an embodiment of the invention.
Fig. 2(a) and 2(b) show the micro-grain structure of the microwave dielectric device manufactured by the embodiment of the invention.
Detailed Description
The invention is explained in detail below with reference to the drawings and with reference to preferred embodiments.
The embodiment of the invention provides a pellet of a microwave dielectric material for injection molding, which comprises 70-90 wt% of the microwave dielectric material and 10-30 wt% of a binder; the microwave dielectric material comprises the following components in percentage by weight: 60 to 70 percent of titanium dioxide, 25 to 35 percent of magnesium oxide, 2 to 8 percent of calcium carbonate, 2 to 8 percent of barium carbonate, 0.1 to 1 percent of niobium pentoxide and 0.1 to 1 percent of bismuth trioxide; the adhesive comprises the following components in percentage by weight: 70-90% of polyformaldehyde, 2-15% of polymethyl methacrylate, 2-15% of polypropylene, 2-15% of ethylene-vinyl acetate copolymer, 2-10% of wax, 1-3% of dioctyl phthalate, 1-3% of dibutyl phthalate and 1-5% of stearic acid.
The embodiment of the invention also provides a preparation method of the microwave dielectric material blank, which comprises the following steps:
s1, preparing a microwave dielectric material and a binder, wherein the microwave dielectric material comprises, by weight, 70% -90% of titanium dioxide, 25% -35% of magnesium oxide, 2% -8% of calcium carbonate, 2% -8% of barium carbonate, 0.1% -1% of niobium pentoxide and 0.1% -1% of bismuth trioxide, and the binder accounts for 10% -30%; the adhesive comprises 70-90% of polyformaldehyde, 2-15% of polymethyl methacrylate, 2-15% of polypropylene, 2-15% of ethylene-vinyl acetate copolymer, 2-10% of wax, 1-3% of dioctyl phthalate, 1-3% of dibutyl phthalate and 1-5% of stearic acid;
s2, banburying and granulating the materials prepared in the step S1;
and S3, performing injection molding on the material obtained in the step S2 to obtain the microwave dielectric material blank.
The manufacturing method of the microwave dielectric device comprises the steps of degreasing and sintering the microwave dielectric material blank prepared by the preparation method of the microwave dielectric material blank to obtain the microwave dielectric device.
Experimental detection shows that the relative dielectric constant epsilon of the microwave dielectric device manufactured by the embodiment of the inventionrQ x f value, temperature coefficient of resonance frequency taufCompared with the traditional method, the method has the advantages that the crystal grains of the sample are compact, fine and uniform.
In a preferred embodiment, the preparation method of the microwave dielectric material blank comprises the following steps:
(1) mixing 70-90% of the microwave dielectric material and 10-30% of the binder by weight percent into pug, automatically shearing the pug into a material with the diameter of 5-10 mm in an internal mixer after the pug is mixed, and preparing for injection molding;
(2) heating and melting the material in a barrel of an injection machine at 150-200 ℃, injecting the melted material into a mold cavity under the pressure of 100-150 Bar, and filling the mold cavity;
(3) and after the mold cavity is filled, conducting heat in the material out through the mold, opening the mold, and taking out the solidified green body, namely the microwave device green body.
Wherein, small block materials of phi 5 mm-phi 10mm can enter the injection machine barrel more easily for injection molding; in order to inject materials into a mold cavity, the materials are heated and melted in a material barrel of an injection machine, the materials are gathered, homogenized and pressurized through the reciprocating motion of a screw, and fluid flows out of a nozzle and passes through a pouring gate, a flow passage and a pouring gate to fill the mold cavity, wherein the setting of process parameters needs to consider the characteristics of microwave medium materials, the composition of a binder, the viscosity of the materials, the working conditions of the mold and the injection machine and other complex factors. The material is completely plasticized in the charging barrel under the mechanical heat action of the external heater and the screw. During the molding process, the pressure is controlled to be increased to inject the material into the mold cavity. The inventor finds a preferable process control mode on the basis of a great deal of experiments: the material is heated and melted in a material barrel of an injection machine at the temperature of 150-200 ℃, the melted material is injected into a mold cavity under the pressure of 100-150 Bar, the mold cavity is filled, the flow rate of the melt is reduced along with the increase of the pressure of the mold cavity, when the mixture is cooled down in the mold, the filling process is finished, and after the mold cavity is filled, the heat in the material is conducted out through the mold and is solidified into a blank.
During injection molding, an in-mold cutting technology can be adopted, the product and the nozzle material are separated in the mold, and the product and the nozzle material are taken out by a manipulator in an automatic mode.
When the die is closed, the sliding blocks on the two sides of the die are connected together through the guide posts, the molten feed is injected into the die cavity, the die cavity is filled, after solidification, the die is opened, the sliding blocks are automatically separated, and the ejector pins eject the product. The required shape or style is formed in one step without processing, thus shortening the manufacturing process and avoiding the adverse phenomena of processing size precision, stress generated by processing, easy breakage of products and the like.
Referring to fig. 1, the method for manufacturing a microwave dielectric device according to the embodiment of the present invention specifically includes the following steps:
and sequentially carrying out acid catalytic degreasing, thermal degreasing and sintering on the green body prepared by the microwave dielectric material green body manufacturing method of the embodiment to obtain the microwave dielectric device.
In a preferred embodiment, the acid-catalyzed degreasing is performed in a nitric acid or oxalic acid state, and is performed at a temperature rise rate of 0.3-1.0 ℃/min to 100-200 ℃ to remove more binders, and the acid-catalyzed degreasing is performed in nitrogen;
in a preferred embodiment, the thermal degreasing is performed under the condition of heating to 150-450 ℃ at a heating rate of 0.2-0.8 ℃/min to remove more binder.
The hot degreasing is to heat the blank in the air to the temperature of volatilization or decomposition of the binder component, so that the binder is heated and decomposed to generate a state change and is converted into a gaseous substance, thereby achieving the purpose of degreasing. When the temperature is lower, partial evaporation and removal are realized, the temperature is raised to be higher than the decomposition temperature of the binder, decomposition reaction is carried out, and more binder is removed. The inventor finds that when the thermal degreasing is carried out under the condition that the temperature is increased to 150-450 ℃ at the temperature increasing speed of 0.2-0.8 ℃/min through a large amount of experiments, the product is not easy to deform or have defects.
In a preferred embodiment, the sintering comprises:
a temperature rising stage: slowly heating, slowly heating to 400-500 ℃ from room temperature at a heating rate of 0.2-0.8 ℃/min, and continuously heating to 850-950 ℃ at a heating rate of 1.0-2.0 ℃/min after the binder is discharged;
and (3) a blank gradual shrinkage stage: continuously heating to 1300-1400 ℃ at a heating rate of 0.5-1.5 ℃/min;
and (3) a heat preservation stage: preserving the heat for 1 to 3 hours at the temperature of between 1300 and 1400 ℃;
and (3) cooling: after the sample is burnt, the temperature is reduced, and the cooling rate is 0.5 ℃/min to 2.0 ℃/min.
Sintering directly determines the final composition, phase distribution, grain size, compactness, size, appearance and properties of the ferrite core. The sintering process includes the steps that proper sintering temperature and sintering curve are determined according to different aspects of sintering equipment, pre-sintering temperature, shrinkage of pre-sintering materials, types and adding proportion of binders, product performance requirements, shapes and sizes, blank loading weight and modes and the like, the inventor finds out the preferable scheme on the basis of a large number of experiments, the temperature rising stage is mainly the volatilization process of water, the binders and lubricants in blanks, the temperature rising stage is slowly raised to avoid the blanks from cracking, the blank gradually shrinks, the temperature rising rate of 0.5 ℃/min-1.5 ℃/min can guarantee good comprehensive performance as the sintering process influences the sizes, uniformity, porosity, distribution and the like of sample grains; keeping the temperature for 1 to 3 hours after reaching the maximum sintering temperature of 1300 to 1400 ℃; in the cooling stage, the control of the cooling rate of 0.5-2.0 ℃/min also contributes to the improvement of the performance and the qualification rate of the product.
Through the preferable sintering process, the product has almost no adhesion, deformation and cracking, and the product has consistent external dimension and performance.
Preferably, the acid-catalyzed degreasing is performed in nitrogen, and the thermal degreasing and sintering are performed in natural air.
The invention is further illustrated by the following more specific examples.
Example 1
The pellet for injection molding comprises the following components in percentage by weight:
70 percent of microwave medium material
30 percent of binder
The microwave dielectric material comprises the following components in percentage by weight:
the adhesive comprises the following components in percentage by weight:
mixing the components according to the weight percentage, placing the mixture into an internal mixer for internal mixing, setting the temperature at 180 ℃, setting the rotating speed of a stirrer at 60rpm, and setting the time at 2 h. After the pug is mixed, the pug is automatically sheared into materials with the diameter of 5mm to 10mm in an internal mixer for standby.
Heating and melting the materials in a charging barrel of an injection machine at 180 ℃, injecting the melted materials into a die cavity under the pressure of 110Bar, and filling the die cavity; and after the mold cavity is filled, conducting heat in the material out through the mold, opening the mold, and taking out the solidified green body, namely the microwave device green body.
Sequentially carrying out acid catalytic degreasing, thermal degreasing and sintering on the green body to obtain the microwave device;
the acid-catalyzed degreasing is performed in a nitric acid or oxalic acid state, and is performed under a condition of raising the temperature to 120 ℃ at a temperature raising rate of 0.5 ℃/min to remove more binder, and the acid-catalyzed degreasing is performed in nitrogen.
The thermal degreasing is performed under a condition of heating up to 450 ℃ at a heating rate of 0.3 ℃/min to remove more binder.
The sintering comprises the following steps:
a temperature rising stage: slowly heating, slowly heating from room temperature to 450 ℃ at a heating rate of 0.5 ℃/min, and continuously heating to 900 ℃ at a heating rate of 1.5 ℃/min after the binder is discharged;
and (3) a blank gradual shrinkage stage: continuously heating to 1320 ℃ at the heating rate of 1.5 ℃/min;
and (3) a heat preservation stage: keeping the temperature at the temperature of 1320 ℃ for 2 h;
and (3) cooling: after the sample is fired, the temperature is reduced, and the cooling rate is 1.5 ℃/min.
Example 2
The pellet for injection molding comprises the following components in percentage by weight:
75 percent of microwave medium material
25 percent of binder
The microwave dielectric material comprises the following components in percentage by weight:
the adhesive comprises the following components in percentage by weight:
mixing the components according to the weight percentage, placing the mixture into an internal mixer for internal mixing, setting the temperature to be 185 ℃, setting the rotating speed of a stirrer to be 60rpm, and setting the time to be 2 hours. After the pug is mixed, the pug is automatically sheared into materials with the diameter of 5mm to 10mm in an internal mixer for standby.
Heating and melting the materials in a charging barrel of an injection machine at 185 ℃, injecting the melted materials into a mold cavity under the pressure of 115Bar, and filling the mold cavity; and after the mold cavity is filled, conducting heat in the material out through the mold, opening the mold, and taking out the solidified green body, namely the microwave device green body.
Sequentially carrying out acid catalytic degreasing, thermal degreasing and sintering on the green body to obtain the microwave device;
the acid-catalyzed degreasing is performed in a nitric acid or oxalic acid state, and is performed under a condition of raising the temperature to 120 ℃ at a temperature raising rate of 0.5 ℃/min to remove more binder, and the acid-catalyzed degreasing is performed in nitrogen.
The thermal degreasing is performed under a condition of heating up to 450 ℃ at a heating rate of 0.3 ℃/min to remove more binder.
The sintering comprises the following steps:
a temperature rising stage: slowly heating, slowly heating from room temperature to 450 ℃ at a heating rate of 0.5 ℃/min, and continuously heating to 900 ℃ at a heating rate of 1.5 ℃/min after the binder is discharged;
and (3) a blank gradual shrinkage stage: continuously heating to 1350 ℃ at the heating rate of 1.5 ℃/min;
and (3) a heat preservation stage: keeping the temperature at 1350 ℃ for 2 h;
and (3) cooling: after the sample is fired, the temperature is reduced, and the cooling rate is 1.5 ℃/min.
Example 3
The pellet for injection molding comprises the following components in percentage by weight:
80 percent of microwave medium material
20 percent of binder
The microwave dielectric material comprises the following components in percentage by weight:
the adhesive comprises the following components in percentage by weight:
mixing the components according to the weight percentage, placing the mixture into an internal mixer for internal mixing, setting the temperature to be 190 ℃, setting the rotating speed of a stirrer to be 60rpm, and setting the time to be 2 hours. After the pug is refined, automatically shearing the pug into materials of phi 5mm to phi 10mm in an internal mixer for later use;
heating and melting the materials in a charging barrel of an injection machine at 190 ℃, injecting the melted materials into a die cavity under the pressure of 120Bar, and filling the die cavity; and after the mold cavity is filled, conducting heat in the material out through the mold, opening the mold, and taking out the solidified green body, namely the microwave device green body.
Sequentially carrying out acid catalytic degreasing, thermal degreasing and sintering on the green body to obtain the microwave device;
the acid-catalyzed degreasing is performed in a nitric acid or oxalic acid state, and is performed under a condition of raising the temperature to 120 ℃ at a temperature raising rate of 0.5 ℃/min to remove more binder, and the acid-catalyzed degreasing is performed in nitrogen.
The thermal degreasing is performed under a condition of heating up to 450 ℃ at a heating rate of 0.30 ℃/min to remove more binder.
The sintering comprises the following steps:
a temperature rising stage: slowly heating, slowly heating from room temperature to 450 ℃ at a heating rate of 0.5 ℃/min, and continuously heating to 900 ℃ at a heating rate of 1.5 ℃/min after the binder is discharged;
and (3) a blank gradual shrinkage stage: continuously heating to 1380 ℃ at the heating rate of 1.5 ℃/min;
and (3) a heat preservation stage: keeping the temperature at 1380 ℃ for 2 h;
and (3) cooling: after the sample is fired, the temperature is reduced, and the cooling rate is 1.5 ℃/min.
The microwave devices produced in the three examples were tested for their performance, in comparison with similar products produced by conventional methods, as shown in the following table:
the microstructure analysis of the sample of the present invention and the similar product produced by the conventional method is performed, as shown in fig. 2(a) and 2(b), where fig. 2(a) is the microstructure of the surface of the sample of the present invention, and fig. 2(b) is the microstructure of the surface of the sample of the similar product produced by the conventional method, and it can be seen from the figures that the crystal grains of the sample of the present invention are dense, fine and uniform.
As can be seen from the results of the tests in examples 1-3, the properties of the products produced from the pellets for injection molding of the microwave dielectric device of the present invention are better than those of the products produced by the conventional methods.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several equivalent substitutions or obvious modifications, which are equivalent in performance or use, should be considered to fall within the scope of the present invention without departing from the spirit of the invention.
Claims (10)
1. The granular material of microwave dielectric material for injection molding is characterized by comprising 70-90 wt% of microwave dielectric material and 10-30 wt% of binder; the microwave dielectric material comprises the following components in percentage by weight: 60 to 70 percent of titanium dioxide, 25 to 35 percent of magnesium oxide, 2 to 8 percent of calcium carbonate, 2 to 8 percent of barium carbonate, 0.1 to 1 percent of niobium pentoxide and 0.1 to 1 percent of bismuth trioxide; the adhesive comprises the following components in percentage by weight: 70-90% of polyformaldehyde, 2-15% of polymethyl methacrylate, 2-15% of polypropylene, 2-15% of ethylene-vinyl acetate copolymer, 2-10% of wax, 1-3% of dioctyl phthalate, 1-3% of dibutyl phthalate and 1-5% of stearic acid.
2. A preparation method of a microwave dielectric material blank is characterized by comprising the following steps:
s1, preparing a microwave dielectric material and a binder, wherein the microwave dielectric material comprises, by weight, 70% -90% of titanium dioxide, 25% -35% of magnesium oxide, 2% -8% of calcium carbonate, 2% -8% of barium carbonate, 0.1% -1% of niobium pentoxide and 0.1% -1% of bismuth trioxide, and the binder accounts for 10% -30%; the adhesive comprises 70-90% of polyformaldehyde, 2-15% of polymethyl methacrylate, 2-15% of polypropylene, 2-15% of ethylene-vinyl acetate copolymer, 2-10% of wax, 1-3% of dioctyl phthalate, 1-3% of dibutyl phthalate and 1-5% of stearic acid;
s2, banburying and granulating the materials prepared in the step S1;
and S3, performing injection molding on the material obtained in the step S2 to obtain the microwave dielectric material blank.
3. The method for preparing a blank according to claim 2, wherein in step S3, the material is melted by heating in an injection machine barrel at 150 ℃ to 200 ℃, and the melted material is injected into the mold cavity at a pressure of 100Bar to 150Bar to fill the mold cavity.
4. A method for preparing a body according to claim 2 or 3, wherein in step S3, after the product and the nozzle material are separated in the mold by using an in-mold nozzle cutting technique, the product is removed from the mold.
5. A method for manufacturing a microwave dielectric device, comprising degreasing and sintering the microwave dielectric material blank prepared by the method of any one of claims 2 to 4 to obtain the microwave dielectric device.
6. A method of manufacturing a microwave dielectric device as claimed in claim 5 wherein the degreasing comprises acid catalyzed degreasing and thermal degreasing in sequence.
7. A method for manufacturing a microwave dielectric device as claimed in claim 6, wherein the acid-catalyzed degreasing is performed by using nitric acid or oxalic acid at a temperature rise rate of 0.3 to 1.0 ℃/min to 100 to 200 ℃.
8. A method of manufacturing a microwave dielectric device as claimed in any one of claims 6 to 7 wherein the thermal degreasing is carried out at a temperature rise rate of from 0.2 ℃/min to 0.8 ℃/min to 150 ℃ to 450 ℃.
9. A method of manufacturing a microwave dielectric device according to any of claims 5 to 8, wherein the sintering comprises:
a temperature rising stage: slowly raising the temperature from room temperature to 400-500 ℃ at a temperature raising rate of 0.2-0.8 ℃/min, and after the binder is discharged, continuing raising the temperature to 850-950 ℃ at a temperature raising rate of 1.0-2.0 ℃/min;
and (3) a blank gradual shrinkage stage: continuously heating to 1300-1400 ℃ at a heating rate of 0.5-1.5 ℃/min;
and (3) a heat preservation stage: preserving the heat for 1 to 3 hours at the temperature of between 1300 and 1400 ℃;
and (3) cooling: cooling at a cooling rate of 0.5 ℃/min to 2.0 ℃/min.
10. A method of manufacturing a microwave dielectric device as claimed in any of claims 6 to 9 wherein the acid-catalysed degreasing is carried out in nitrogen; the thermal degreasing and the sintering are both performed in air.
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