CN112645680B - Calcium phosphate-based cement encapsulating material and manufacturing method thereof - Google Patents

Calcium phosphate-based cement encapsulating material and manufacturing method thereof Download PDF

Info

Publication number
CN112645680B
CN112645680B CN202011563028.8A CN202011563028A CN112645680B CN 112645680 B CN112645680 B CN 112645680B CN 202011563028 A CN202011563028 A CN 202011563028A CN 112645680 B CN112645680 B CN 112645680B
Authority
CN
China
Prior art keywords
calcium phosphate
cement
based cement
encapsulating material
polyimide fibers
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202011563028.8A
Other languages
Chinese (zh)
Other versions
CN112645680A (en
Inventor
刘盼
高涵彦
张靖
樊嘉杰
张国旗
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guanghua Lingang Engineering Application Technology Research and Development Shanghai Co Ltd
Original Assignee
Guanghua Lingang Engineering Application Technology Research and Development Shanghai Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guanghua Lingang Engineering Application Technology Research and Development Shanghai Co Ltd filed Critical Guanghua Lingang Engineering Application Technology Research and Development Shanghai Co Ltd
Priority to CN202011563028.8A priority Critical patent/CN112645680B/en
Priority to PCT/CN2020/141292 priority patent/WO2022134163A1/en
Publication of CN112645680A publication Critical patent/CN112645680A/en
Application granted granted Critical
Publication of CN112645680B publication Critical patent/CN112645680B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/34—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
    • C04B28/344—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00939—Uses not provided for elsewhere in C04B2111/00 for the fabrication of moulds or cores
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/34—Non-shrinking or non-cracking materials
    • C04B2111/343—Crack resistant materials

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention provides a calcium phosphate-based cement encapsulating material, wherein nano polyimide fibers are uniformly distributed in calcium phosphate-based cement, and the mass fraction of the nano polyimide fibers is 1-10%. And the calcium phosphate-based cement is used as a basic packaging material, so that the cost is reduced. The cost of the cement is lower than that of any system in the prior art; the encapsulating material system can resist the high temperature of 350 ℃; and the hydration process of the cement is improved by adding the nano polyimide fiber, and the porosity is reduced. After the cement has finally set, the possibility of crack formation is reduced, and the water mist and salt mist resistance of the cement is improved.

Description

Calcium phosphate-based cement encapsulating material and manufacturing method thereof
Technical Field
The invention relates to the field of packaging materials, in particular to a calcium phosphate-based cement encapsulating material and a manufacturing method thereof.
Background
With the rapid development of power electronic systems, the demand of global energy interconnection and the introduction of ubiquitous power internet of things, the performance of power electronic devices based on Si (silicon) has reached its theoretical limit. Driven by various challenges and practical requirements, there is a continuing need to improve the switching and turn-on performance of devices, and wide bandgap semiconductors are therefore emerging. However, the current electronic packaging system is developed based on Si (silicon) devices, and when the wide bandgap semiconductor device is used to replace the silicon device and the development is towards high voltage, high temperature and high frequency, the original packaging system is not suitable, and the packaging material has become an important bottleneck for restricting the performance of the wide bandgap semiconductor device.
As for the encapsulating material, epoxy resin or silica gel is used in Si (silicon) devices, and as organic substances, they have a common defect of not withstanding high temperature, and the highest tolerable working temperature is only 175 ℃. In operation, wide bandgap semiconductor devices can often reach temperatures above 250 ℃ and even higher. Therefore, it is urgent to find a high temperature resistant potting material. Meanwhile, the cost problem needs to be considered, the development of new materials usually means the increase of the cost, and the development cost of epoxy resin or silica gel is stable and relatively low after many years, so that the development of high-temperature-resistant low-cost encapsulating materials is a necessary condition for the practical application of wide-bandgap semiconductors.
In the pouring sealant industry, there are three major potting materials, epoxy resin pouring sealant, polyurethane pouring sealant and organic silicon pouring sealant. The three pouring sealant materials are researched, developed and improved for decades, and account for more than 99% of the pouring sealant industry. Epoxy resin pouring sealant, the repairability is not good after the potting; the high-temperature and low-temperature resistant performance cannot be simultaneously achieved, the high-temperature resistance is generally good, the low-temperature resistance is poor, and vice versa; the heat productivity is large in the curing process, and the impact damage resistance is poor. The polyurethane pouring sealant has certain toxicity and general temperature resistance, and the temperature of the polyurethane pouring sealant is generally not more than 100 ℃. The mixture should be vacuum-sealed and filled with a large amount of bubbles. The curing process is exothermic and some stress is generated. The chemical structure of the film is damaged by long-time ultraviolet irradiation, and the weather resistance is poor. The organosilicon pouring sealant has the defects of poor adhesion to materials and higher unit price. The high temperature resistance requires special modulation.
If cement casting glues are used, a large number of the above problems can be solved, but cement materials also have their own disadvantages. For example, pores may be present, and cracks may be generated in the case of long-term use. The metal ions in the cement may migrate under the action of the electric field to cause the cement to crack. While the cement may chemically react with the metal layer on the device surface. Therefore, the cement material applied to the encapsulation of the wide bandgap semiconductor needs to be modified.
In the prior art, researches on the encapsulating materials still focus on the modification of the original mature material system. Namely, various inorganic and organic fillers are utilized to modify epoxy resin and organic silicon rubber, so that the modified material has excellent properties. For example, the potting material is made of aluminum oxide and silicone rubber, and can conduct heat and insulate. The encapsulating material with high resistance and good heat conduction is prepared by mixing aluminum nitride, aluminum oxide and epoxy resin.
Disclosure of Invention
The invention aims to solve the technical problem of providing a calcium phosphate-based cement encapsulating material and a manufacturing method thereof, which can resist cracking and corrosion.
In order to solve the problems, the invention provides a calcium phosphate-based cement encapsulating material, wherein nano polyimide fibers are uniformly distributed in the calcium phosphate-based cement, and the mass fraction of the nano polyimide fibers is 1-10%.
In order to solve the problems, the invention provides a method for manufacturing a calcium phosphate-based cement encapsulating material, which comprises the following steps: dissolving nano polyimide fibers in water to form fiber liquid; and continuously adding the dissolved fiber liquid in the hydration process of the calcium phosphate-based cement, stirring and uniformly mixing to obtain the calcium phosphate-based cement encapsulating material for encapsulation, wherein the mass fraction of the polyimide is 1-10%.
In order to solve the problems, the invention provides a method for manufacturing a calcium phosphate-based cement encapsulating material, which comprises the following steps: adding water into potassium hydrogen phosphate powder, calcium oxide powder and nano polyimide fiber, and stirring and mixing together; and hydrating the calcium phosphate-based cement by adopting water mixed with the substances to obtain the calcium phosphate-based cement encapsulating material for encapsulation, wherein the mass fraction of the polyimide is 1-10%.
The technical scheme adopts the calcium phosphate-based cement as the basic packaging material, thereby reducing the cost. The cost of the cement is lower than that of any system in the prior art; the encapsulating material system can resist the high temperature of 350 ℃; and the hydration process of the cement is improved by adding the nano polyimide fiber, and the porosity is reduced. After the cement has finally set, the possibility of crack formation is reduced, and the water mist and salt mist resistance of the cement is improved.
Drawings
Fig. 1 is a microstructure diagram of cement according to an embodiment of the present invention, illustrating the water mist resistance principle.
Detailed Description
The following will describe in detail specific embodiments of a calcium phosphate-based cement potting material and a method for manufacturing the same according to the present invention.
The concrete embodiment provides a calcium phosphate-based cement encapsulating material, wherein nanometer polyimide fibers are uniformly distributed in the calcium phosphate-based cement, and the mass fraction of the nanometer polyimide fibers is 1-10%. Preferably, the nano polyimide fiber has a fiber length ranging from 30 to 80 micrometers and a fiber diameter ranging from 30 to 200 nanometers.
The cement material can be obtained by two modes, one mode is a mixing mode during stirring, namely, the nano polyimide fiber is dissolved in water to form fiber liquid; and continuously adding the dissolved fiber liquid in the hydration process of the calcium phosphate-based cement, stirring and uniformly mixing to obtain the calcium phosphate-based cement encapsulating material for encapsulation, wherein the mass fraction of the polyimide is 1-10%. Preferably, the stirring temperature is 25-100 ℃ and the stirring time is 10-60 minutes.
The other is mixing before the cement hydration process (without adding water), namely adding water into potassium hydrogen phosphate powder, calcium oxide powder and the nano polyimide fiber, and stirring and mixing together; and hydrating the calcium phosphate-based cement by adopting water mixed with the substances to obtain the calcium phosphate-based cement encapsulating material for encapsulation, wherein the mass fraction of the polyimide is 1-10%.
The above mode adopts calcium phosphate-based cement as a basic packaging material, so that the cost is reduced. The cost of the cement is lower than that of any system in the prior art; the encapsulating material system can resist the high temperature of 350 ℃; and the hydration process of the cement is improved by adding the nano polyimide fiber, and the porosity is reduced. After the cement has finally set, the possibility of crack formation is reduced, and the water mist and salt mist resistance of the cement is improved.
The principle of the water mist resistance of the cement in the technical scheme is shown in the attached drawing 1, irregular balls and large balls are cement particles, and strips are polyimide. The polyimide improves the porosity of the cement formed during hydration, thereby reducing the porosity. Without the polyimide nanofibers, the nuclei of the cement that are first formed during hydration form on the surface of the large spherical cement particles, blocking further dissolution of the large spherical cement particles. So that the diameters of finally formed cement particles are different, the distance between the spheres is different, and the void ratio is high. If the polyimide nanofibers are present, the surface of the polyimide nanofibers provide attachment points for the primarily formed cement nuclei, which can accumulate on the surface of the polyimide and then gradually fuse to form large spheres and then fall off the surface of the polyimide. Providing another mechanism for the hydration process of cement. The cement crystal nucleus formed by the mechanism has average diameter and higher hydration speed, and the balls are compact, so that the porosity is reduced. In addition, the added polyimide can fill the gaps between the large spheres and between the small spheres and the large spheres, so that the porosity is reduced. The porosity can be reduced by 50-70%. The essential reason is that the polyimide fibers provide a sink point for the crystal nuclei, while the polyimide itself can fill a part of the voids.
The principle of the cement salt fog resistance in the technical scheme is that calcium phosphate cement does not react with salt fog per se, and polyimide does not react with salt fog. At the same time, salt spray is difficult to enter the interior of the module through the gap because of the reduced porosity.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (5)

1. The calcium phosphate-based cement encapsulating material is characterized in that nano polyimide fibers are uniformly distributed in the calcium phosphate-based cement, wherein the mass fraction of the nano polyimide fibers is 1% -10%, the fiber length range of the nano polyimide fibers is 30-80 micrometers, and the fiber diameter range is 30-200 nanometers.
2. The method for manufacturing the calcium phosphate-based cement encapsulating material is characterized by comprising the following steps of:
dissolving nano polyimide fibers in water to form fiber liquid;
and continuously adding the dissolved fiber liquid in the process of hydrating the calcium phosphate-based cement, stirring and uniformly mixing to obtain the calcium phosphate-based cement encapsulating material for encapsulating, wherein the mass fraction of the nano polyimide fibers is 1-10%, the fiber length range of the nano polyimide fibers is 30-80 microns, and the fiber diameter range is 30-200 nanometers.
3. The method of claim 2, wherein the temperature of the agitation is in the range of 25-100 degrees celsius and the time of agitation is in the range of 10-60 minutes.
4. The method for manufacturing the calcium phosphate-based cement encapsulating material is characterized by comprising the following steps of:
adding water into potassium hydrogen phosphate powder, calcium oxide powder and nano polyimide fiber, and stirring and mixing together;
and hydrating the calcium phosphate-based cement by adopting water mixed with the substances to obtain the encapsulated calcium phosphate-based cement encapsulating material, wherein the mass fraction of the nano polyimide fibers is 1-10%, the fiber length range of the nano polyimide fibers is 30-80 microns, and the fiber diameter range is 30-200 nanometers.
5. The method of claim 4, wherein the temperature of the agitation is in the range of 25-100 degrees Celsius and the time of agitation is in the range of 10-60 minutes.
CN202011563028.8A 2020-12-25 2020-12-25 Calcium phosphate-based cement encapsulating material and manufacturing method thereof Active CN112645680B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202011563028.8A CN112645680B (en) 2020-12-25 2020-12-25 Calcium phosphate-based cement encapsulating material and manufacturing method thereof
PCT/CN2020/141292 WO2022134163A1 (en) 2020-12-25 2020-12-30 Calcium phosphate-based cement potting material and preparation method therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011563028.8A CN112645680B (en) 2020-12-25 2020-12-25 Calcium phosphate-based cement encapsulating material and manufacturing method thereof

Publications (2)

Publication Number Publication Date
CN112645680A CN112645680A (en) 2021-04-13
CN112645680B true CN112645680B (en) 2022-03-08

Family

ID=75363004

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011563028.8A Active CN112645680B (en) 2020-12-25 2020-12-25 Calcium phosphate-based cement encapsulating material and manufacturing method thereof

Country Status (2)

Country Link
CN (1) CN112645680B (en)
WO (1) WO2022134163A1 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114149243B (en) * 2021-12-21 2023-04-07 厦门钜瓷科技有限公司 Inorganic encapsulating material, preparation method and application thereof, and temperature sensor
CN115403353A (en) * 2022-06-28 2022-11-29 复旦大学 Cement potting material and method for producing same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104745141A (en) * 2015-03-04 2015-07-01 深圳广恒威科技有限公司 Bi-component condensed type organic silicon pouring sealant as well as preparation method and application thereof
CN109999220A (en) * 2019-03-01 2019-07-12 西南交通大学 The preparation method of fiber reinforced calcium orthophosphate base bone renovating material for 3D printing

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0360451A (en) * 1989-07-25 1991-03-15 Natl Inst For Res In Inorg Mater Calcium phosphate hydraulic cement composition
CN103877621B (en) * 2014-04-08 2015-07-08 广东药学院 Electrospun fiber-reinforced calcium phosphate bone cement composite material and application thereof
CN107137771B (en) * 2017-05-02 2020-02-07 南京医科大学附属口腔医院 Nano calcium phosphate bone cement and preparation method thereof
CN107899084A (en) * 2017-10-23 2018-04-13 广州润虹医药科技股份有限公司 A kind of bone cement and preparation method
JP6715270B2 (en) * 2018-02-02 2020-07-01 大王製紙株式会社 Cement composition and cured product thereof
CN108744030B (en) * 2018-07-20 2021-01-15 西安理工大学 Injection type piezoelectric bone cement and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104745141A (en) * 2015-03-04 2015-07-01 深圳广恒威科技有限公司 Bi-component condensed type organic silicon pouring sealant as well as preparation method and application thereof
CN109999220A (en) * 2019-03-01 2019-07-12 西南交通大学 The preparation method of fiber reinforced calcium orthophosphate base bone renovating material for 3D printing

Also Published As

Publication number Publication date
CN112645680A (en) 2021-04-13
WO2022134163A1 (en) 2022-06-30

Similar Documents

Publication Publication Date Title
CN112645680B (en) Calcium phosphate-based cement encapsulating material and manufacturing method thereof
CN106519581B (en) A kind of high heat conduction low viscosity epoxy resin composite material and preparation method and application
JP6545193B2 (en) Semiconductor module comprising sealing compound covering at least one semiconductor component
CN106164142B (en) Conductive and heat-conductive paste composition and using the composition reduce percolation threshold and improve exceed seep conductive performance method
US7799849B2 (en) Method to fabricate self-healing material
WO2009140836A1 (en) A self repairing concrete containing microcapsules of polyurea resin and producing method thereof
CN108641645A (en) A kind of encapsulating semiconductor packaging plastic and preparation method thereof
WO2020119756A1 (en) Thermal interface material and preparation method therefor
CN105969277A (en) Heat-dissipating pouring sealant for packaging electronic devices
CN111732108A (en) Porous amorphous silicon dioxide powder and preparation method and application thereof
CN102212269A (en) Insulative potting composite material with high thermal conductivity and preparation method thereof
CN113004708B (en) Asphalt anti-stripping agent and preparation method thereof
EP2167577A1 (en) Thermally conductive underfill formulations
CN112250996A (en) Micro-nano epoxy resin electronic packaging material and preparation method and application thereof
CN106634812A (en) Organic silicon resin pouring sealant with high thermal conductivity and low viscosity for PCB (Printed Circuit Board)
CN103497717B (en) A kind of LED heat-conductive solid crystal glue binder and preparation method thereof
CN115403353A (en) Cement potting material and method for producing same
CN103602308A (en) Pressure-sensitive adhesion type double-component low-thermal-resistance room-temperature curing organic silicon thermal conductive adhesive
CN106479431A (en) A kind of little PCB organic silicon electronic potting adhesive of cure shrinkage
CN104559882B (en) A kind of liquid crystal type epoxy underfill and preparation method thereof
CN102352025B (en) Preparation method of silica modified epoxy resin curing agent and varnish
CN104672496A (en) Insulating heat-conducting graphite micro powder with core-shell structure as well as preparation method and application thereof
CN113999617A (en) Method for preparing inorganic heat-conducting glue by using etched diamond micro powder as filler
CN107226639A (en) A kind of epoxy resin grouting material and preparation method thereof
KR20150116717A (en) Insulation coating composition and manufacturing method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant