CN113135747A - Preparation method of microwave ferrite - Google Patents
Preparation method of microwave ferrite Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 103
- 238000000034 method Methods 0.000 claims abstract description 48
- 238000012545 processing Methods 0.000 claims abstract description 31
- 239000000047 product Substances 0.000 claims abstract description 26
- 239000011265 semifinished product Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 25
- 239000000463 material Substances 0.000 abstract description 22
- 239000000758 substrate Substances 0.000 abstract description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
- 239000002223 garnet Substances 0.000 description 5
- 238000007781 pre-processing Methods 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 4
- 229910052596 spinel Inorganic materials 0.000 description 4
- 239000011029 spinel Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005350 ferromagnetic resonance Effects 0.000 description 3
- 238000009766 low-temperature sintering Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
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- 239000012467 final product Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
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- 230000002159 abnormal effect Effects 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 230000005484 gravity Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of microwave ferrite, belonging to the technical field of ferrite.A powder material is molded to obtain a green body in the step (A); (B) sintering the green body to obtain a semi-finished blank; (C) processing the semi-finished blank to obtain a semi-finished product; (D) sintering the semi-finished product to obtain a ferrite matrix finished product; the semi-finished blank is ground and processed by step-by-step sintering and two-step sintering, so that the problem that a substrate with a special structure required by a novel microwave ferrite device is difficult to produce and process is solved; compared with the existing one-step sintering method, the method avoids directly and complexly processing the polycrystalline cooked blank with high hardness and brittleness, has mass production capacity, improves the yield by reducing the processing stress damage, greatly reduces the processing difficulty of the special-shaped ferrite substrate, and is favorable for the low-cost and mass production of microwave devices of special-shaped substrates.
Description
Technical Field
The invention relates to the technical field of microwave ferrite, in particular to a preparation method of microwave ferrite.
Background
At present, in order to meet the design requirements of microwave ferrite devices, a ferrite substrate with a special structure needs to be provided, but due to the fact that ferrite has the characteristics of high hardness and high brittleness, special-shaped processing is difficult to perform in a grinding mode, and meanwhile, the ferrite is not conductive and cannot be subjected to linear cutting.
In order to solve the above problems, the production is generally performed by making molds of different shapes, but the following problems exist in this way: the grinding is difficult, the processing difficulty is high, the processing precision is difficult to guarantee, the production efficiency is low, the deformation and the damage result in low yield, and the production cost is high.
In the application field of 5G, the nested ferrite substrate becomes a hot door, and especially under the condition that the size precision needs to be higher, the size change rate of a sintered product is difficult to be uniform and consistent only by the design of a grinding tool under the existing process conditions, so that the size of a special-shaped finished product is difficult to control with high precision.
The ferrite material, especially the garnet type ferrite material, has a high sintering temperature (generally above 1300 ℃), and the optimal sintering temperature area is narrow, and the performance of the ferrite material is greatly influenced by the sintering process, so that high-temperature precise sintering equipment is required.
In addition, a large amount of organic adhesive is added during the granulation of the ferrite material, and the gasified adhesive has adverse effect on high-temperature sintering equipment and shortens the service life of the high-temperature sintering equipment; meanwhile, precise sintering equipment is often accompanied with good air tightness, and the volatilized glue gas cannot escape and is retained in the sintering equipment in the sintering process, so that the ferrite is polluted by reverse osmosis of glue elements in the sintering process, and the electromagnetic performance of the ferrite is greatly damaged.
At present, the disclosed two-step sintering method generally comprises the steps of firstly carrying out short-time heat preservation at a higher temperature and then reducing the temperature to the normal sintering temperature for sintering; the sintering method cannot change sintering equipment, cannot process products midway, and is essentially one-time sintering, for example, chinese patent application with publication number CN103964830A and the name of "a method for preparing permanent magnetic ferrite by low-temperature sintering" discloses two-time sintering, and is a method for preparing permanent magnetic ferrite by low-temperature sintering and then higher-temperature sintering, but those skilled in the art know that the preparation process of ferrite comprises the following steps: the first sintering of the two-time sintering disclosed by the patent application belongs to a 'pre-sintering' process, the process is broken and then molded after the first sintering, and the first sintering of the process belongs to a sintering process of a molded product and is only subjected to size processing subsequently, so that the process is not molded again and the sintering requirements of large-size and special-shaped microwave ferrite materials are difficult to meet.
Disclosure of Invention
The present invention aims at providing a method for preparing microwave ferrite to solve the above problems.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of microwave ferrite comprises the following steps:
(A) molding the powder to obtain a green body;
(B) sintering the green body obtained in the step (A) to obtain a semi-finished blank;
(C) processing the semi-finished blank obtained in the step (B) to obtain a semi-finished product;
(D) sintering the obtained semi-finished product to obtain a ferrite matrix finished product;
wherein, the step (B) and the step (C) are circulated for one or more times;
the invention adopts a low-temperature and high-temperature two-step sintering method, can completely volatilize and remove adhesive and the like in the first low-temperature sintering of the step (B), prevents harmful atmosphere from generating adverse effect on high-temperature and high-precision equipment, particularly lightens the corrosion action of the harmful atmosphere on a heater body and a heat insulation layer of the equipment, can effectively prolong the replacement period of the heater and prolong the service life of the equipment; the sintering performance of the product can be promoted by effectively removing the adhesive and optimizing the sintering surface area of the product, and the adhesive has obvious improvement effect on large-size products; high-precision atmosphere sintering equipment often has good leakproofness, and after the volatile components such as adhesive are removed through the first step sintering, the finished product abnormal sintering caused by reverse osmosis products of the volatile substances during sintering in the precision equipment can be prevented. Meanwhile, the occupied time of the low-temperature section of the precision equipment can be reduced by using low-temperature equipment with poor performance through step-by-step sintering, the effective utilization rate of the precision equipment is improved, and the residence time of the equipment heating body in an oxidation temperature interval is reduced to protect the equipment heating body; the material can obtain certain processing strength after being sintered at a lower temperature, and can be processed, so that the problem that the finished product is easy to crack due to high hardness and extremely poor toughness during processing is solved.
Semi-finished products with different specifications can be obtained through the processing in the step (C), and compared with the polycrystalline ferrite which is directly processed and has high hardness and high brittleness, the semi-finished blank which is obtained through the one-time sintering in the step (B) and has lower hardness and better toughness is more beneficial to being processed into the ferrite with complex appearance characteristics, and the processing difficulty is lower.
The material type suitable for the invention is spinel, garnet or magnetoplumbite type ferrite material, or dielectric ceramic material matched with the spinel, garnet or magnetoplumbite type ferrite material.
The invention is especially suitable for processing the special-shaped ferrite substrate. Due to the existence of the preprocessing procedure, the material forming blank and the finished product can have larger shape access, namely, the material forming blank can be formed into a simple shape, and the requirement on high-grade forming equipment is reduced.
By adopting the processing mode of the invention, the production and processing capacity foundation can be provided for the special-shaped nested ferrite substrate.
As a preferred technical scheme: in the step (A), the powder forming pressure is controlled to be 10 MPa-300 MPa.
As a preferred technical scheme: in the step (B), the sintering temperature is 600-1200 ℃, and the heat preservation time is 2-5 hours.
As a preferred technical scheme: in the step (C), the processing method is grinding. Grinding is an effective way to improve dimensional accuracy.
As a preferred technical scheme: in the step (D), the sintering temperature is 800-1500 ℃, and the time is 4-15 hours.
As a preferred technical scheme: different sintering equipment is adopted in the steps (B) and (D). Sintering atmosphere can be improved by replacing sintering equipment, precision equipment and sintered products can be effectively protected, and stability and reliability of the products are further improved.
Compared with the prior art, the invention has the advantages that: the semi-finished blank is ground and processed by step-by-step sintering and two-step sintering, so that the problem that a substrate with a special structure required by a novel microwave ferrite device is difficult to produce and process is solved; the invention can effectively protect the precise sintering equipment and improve the electromagnetic performance of the finished product by replacing different sintering equipment in the two sintering processes. Compared with the existing one-step sintering method, the method avoids directly and complexly processing the polycrystalline cooked blank with high hardness and brittleness, has mass production capacity, improves the yield by at least 15 percent by reducing processing stress damage, greatly reduces the processing difficulty of the special-shaped ferrite substrate, and is favorable for low-cost and mass production of microwave devices of special-shaped substrates.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic view showing the production of a ferrite substrate according to example 1 of the present invention;
FIG. 3 is a schematic diagram of the ferrite substrate of example 1 of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings.
A preparation method of microwave ferrite, the corresponding ferrite magnetic material structure is garnet type, spinel type and magnetoplumbite type ferrite, and the sintering temperature is 800-1500 ℃. The ferrite substrate can lead the microwave to show the nonreciprocal characteristic in the transmission process, and can be widely applied to manufacturing microwave annular transmission and phase-shifting devices. In order to make the semi-finished blank have enough strength to be applied to grinding processing and not make the processing difficult due to too high hardness, the sintering temperature in the step (B) needs to be accurately controlled; the finished pre-finished green article is further densified during the sintering process of step (D), exhibiting dimensional shrinkage. Therefore, the pre-processing technological parameters need to be accurately controlled according to the actual situation, and the size of the cooked blank is lower than the required size due to excessive processing amount, so that the blank is scrapped; the allowance left after preprocessing is too large, so that the risk of workpiece damage is increased due to high-strength supplementary processing, and the significance of preprocessing is reduced; further, a cooked blank with the shape and the size meeting the product requirements can be directly obtained after sintering is finished by accurately controlling the shrinkage process and the shrinkage rate of the sample in the sintering process, or further, simple processing is carried out to ensure that the shape and the size meet the product requirements; repeating the operation process of the step (B) and the step (C), and preprocessing for multiple times under different strengths to adapt to various processing requirements, as shown in figure 1.
Example 1:
referring to fig. 2, a method for preparing a microwave ferrite substrate includes the following steps:
(A) using certain garnet ferrite powder, forming under 100MPa to obtain 50 pieces of disc-shaped ferrite green bodies with the diameter phi of 20mm and the thickness of 2.4mm by dry forming;
(B) sintering the green body at a temperature lower than the optimal sintering process temperature, setting the sintering temperature to be 1300 ℃, and obtaining a semi-finished ferrite block with the size diameter phi of 18.3mm and the thickness of 2.2 mm;
(C) firstly, the plane of the above-mentioned semi-cooked ferrite material block body is processed to 1.75mm, the plane-processed block bodies are arranged, and adhered into a column body, and then processed again so as to make its external diameter size be phi 17.62±0.02mm, selecting a diameter on the surface of the substrate as a processing coordinate, and processing grooves with the width of 7.16 mm and the depth of 2.75mm inwards from the intersection point of the diameter and the outer diameter ring by taking the diameter as a bisector; will addCleaning and drying the machined workpiece to obtain a semi-finished product;
(D) c, sintering the semi-finished product processed in the step C at the optimal sintering temperature of 1450 ℃, and supporting the blank by using alumina isolation powder to prevent the blank from softening at high temperature and deforming under the influence of gravity; detecting the size of the cooked blank as diameter 16±0.03mm, thickness 1.59± 0.03mm, groove width 6.5±0.03mm, groove depth 2.5±0.03mm, the alignment of the bisector of the groove is not deviated. Further grinding the flat surface of the cooked blank to a thickness of 1.5±0.02mm, obtained to phi 16±0.03*1.5±0.02mm, symmetrical groove width 6.5±0.03Depth 2.5±0.03The mm products are 44 pieces in total, and the yield is about 88%; in contrast, the yield of the conventional one-step sintering process is about 70%.
The sintering temperature of the embodiment is 1300 ℃, materials of the same type often have different optimal sintering temperatures due to different doping types, and the optimal sintering temperature of the materials of the embodiment adopting conventional one-time sintering is 1450 ℃;
the final product of test example 1 has a ferromagnetic resonance linewidth of 2.86kA/m, and compared with the linewidth Δ H obtained by one-time sintering at 1450 ℃ in the conventional method, the linewidth Δ H is 3.50kA/m, and it can be seen that the linewidth value of the product obtained by the step-by-step sintering at 1300 ℃ is better than the result obtained by one-time optimal temperature sintering.
Example 2:
referring to fig. 3, a method for preparing a microwave ferrite substrate includes the following steps:
(A) using certain spinel ferrite powder, and forming under the forming pressure of 100MPa to obtain 100 annular ferrite green bodies with the outer diameter phi of 32mm, the inner diameter phi of 12mm and the thickness of 2.4mm by dry forming;
(B) sintering the green body at a temperature lower than the optimal sintering process temperature, wherein the sintering temperature is set to be 800 ℃; obtaining a semi-cooked ferrite annular block with the size of phi 30.21mm in outer diameter and phi 11.33mm in inner diameter and the thickness of 2.27 mm;
(C) firstly, the plane of the semi-finished ferrite material block is processed to 1.75±0.02mm, orderly arranging the blocks after plane processing, adhering the blocks into a cylinder, and processing again to obtain a cylinder with the center of the face being the same as that of the inner diameter and the center of the circleThe center and side length are 28.89±0.02A regular hexagon of mm. The inner diameter is expanded to phi 13.33 from the center of the inner diameter to the outside±0.02Simultaneously, one diameter of the inner ring of the substrate is selected to be a bisector, and two circles 5.55 away from the circle center are left in the inner diameter processing process±0.02mm and length of 5.55±0.02The protrusions with mm are centrosymmetric according to the center of the circle. And cleaning and drying the processed workpiece.
(D) And C, sintering the semi-finished product processed in the step C at the optimal sintering temperature of 1200 ℃, and controlling the shrinkage process to prevent deformation. Detecting the size of the cooked blank as side length 26±0.03mm, inner diameter 12±0.03mm, thickness 1.58±0.03mm, convex part width 5±0.03mm, circle center distance 5±0.03mm and is centrosymmetric around the center of the circle. Further grinding the flat surface of the cooked blank to a thickness of 1.5±0.02mm. To obtain an edge length of 26±0.02mm regular hexagon, thickness 1.5±0.02mm, inner diameter 12±0.03mm, centrosymmetric bulge size: length 5±0.03mm, 5 from the center of the face±0.03The total number of mm finished products is 90, and the yield reaches 90%.
The sintering temperature of the embodiment is 800 ℃, materials of the same type often have different optimal sintering temperatures due to different doping types, and the optimal sintering temperature of the materials of the embodiment adopting conventional one-time sintering is 1200 ℃;
the final product of test example 2 had a ferromagnetic resonance linewidth of 19.41kA/m, whereas the linewidth Δ H obtained by one sintering at a temperature of 1200 ℃ was 21.25kA/m, which shows that the linewidth values of the product obtained by stepwise sintering at 1200 ℃ are better than those obtained by one optimum temperature sintering.
Example 3 of implementation:
a preparation method of a microwave ferrite substrate comprises the following steps:
(A) using ferrite powder of a certain type, and molding under the pressure of 100MPa to obtain a ferrite green compact with the dimensions of 51mm in length, 41mm in width and 33mm in height by dry molding;
(B1) sintering the green body at a temperature lower than the optimal sintering process temperature, wherein a silicon carbide rod sintering furnace is adopted in the sintering, and the sintering temperature is set to be 600 ℃; obtaining a ferrite block without adhesive and moisture, the size of which is 50mm in outer diameter length and 40mm in width and 32mm in height;
(B2) and cooling the ferrite material block in the last step along with the furnace, transferring the cooled ferrite material block into a high-precision silicon-molybdenum rod sintering furnace, setting the secondary sintering temperature to 1380 ℃, and obtaining the ferrite block with the length of 43.8, the width of 35.2 and the height of 28.
(C) The ferrite block obtained in B2 was cut into ferrite pieces 42.5mm long, 33.4mm wide and 1.12 mm thick. And cleaning and drying the processed workpiece.
(D) And D, sintering the ferrite sheet processed in the step C at the optimal sintering temperature of 1400 ℃, and controlling the shrinkage process to prevent deformation. Determination of cooked-base size as Length 42±0.03mm, width 33±0.03mm, thickness 1.1±0.03A ferrite sheet of mm formed by further polishing the surface of the substrate to a thickness of 1.0±0.02mm. To a dimension of 42±0.03mm, width 33±0.03mm, thickness 1.00±0.03And (5) obtaining a mm finished product.
The sintering temperature of the embodiment is 600 ℃, materials of the same type often have different optimal sintering temperatures due to different doping types, and the optimal sintering temperature of the materials of the embodiment adopting conventional one-time sintering is 1400 ℃;
the finished product of the test example 3 has a ferromagnetic resonance line width Δ H of 1.99kA/m, which is 2.86kA/m compared with the line width Δ H obtained by one-time sintering at 1400 ℃, and it can be seen that the line width value of the product obtained by step-by-step sintering at 600 ℃ is obviously better than the result of one-time optimal temperature sintering, which is obviously improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The preparation method of the microwave ferrite is characterized by comprising the following steps of:
(A) molding the powder to obtain a green body;
(B) sintering the green body obtained in the step (A) to obtain a semi-finished blank;
(C) processing the semi-finished blank obtained in the step (B) to obtain a semi-finished product;
(D) sintering the obtained semi-finished product to obtain a ferrite matrix finished product;
wherein the steps (B) and (C) are performed in one or more cycles.
2. The method for preparing microwave ferrite according to claim 1, wherein the method comprises the following steps: in the step (A), the powder forming pressure is controlled to be 10 MPa-300 MPa.
3. The method for preparing microwave ferrite according to claim 1, wherein the method comprises the following steps: in the step (B), the sintering temperature is 600-1200 ℃, and the heat preservation time is 2-5 hours.
4. The method for preparing microwave ferrite according to claim 1, wherein the method comprises the following steps: in the step (C), the processing method is grinding.
5. The method for preparing microwave ferrite according to claim 1, wherein the method comprises the following steps: in the step (D), the sintering temperature is 800-1500 ℃, and the time is 4-15 hours.
6. The method for preparing microwave ferrite according to claim 1, wherein the method comprises the following steps: different sintering equipment is adopted in the steps (B) and (D).
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1811761A1 (en) * | 1968-03-01 | 1969-10-16 | Rca Corp | Process for producing a ferrite laminate |
| US5256242A (en) * | 1989-04-28 | 1993-10-26 | Ngk Insulators, Ltd. | Method of manufacturing ferrite crystals |
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