CN109294465A - A kind of room temperature thermal control flexible macromolecule matrix PTC material and preparation method thereof - Google Patents
A kind of room temperature thermal control flexible macromolecule matrix PTC material and preparation method thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
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- C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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- C08J2391/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
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- C09J2301/124—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present on both sides of the carrier, e.g. double-sided adhesive tape
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- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
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Abstract
The invention discloses a kind of room temperature thermal control flexible macromolecule matrix PTC materials and preparation method thereof, the material includes block copolymer, phase transformation matrix and conductive filler, wherein the mass ratio of the block copolymer and phase transformation matrix is (20: 80)~(40: 60), and the mass ratio of the conductive filler is less than 80%；Block copolymer is added as backing material in the present invention in the composite material of paraffin and graphite powder or conductive black, and by adjusting the formula of each component, so that the Curie temperature that the material prepared generates PTC effect is -10~40 DEG C, have preferable flexible and is able to achieve filming, active temperature control and other room temperature thermal control fields that can be applied to electronic device, compensating for not having for current ambient temperature thermal control ptc material flexibility and can not be prepared into the major defect of film.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of room temperature thermal control flexible macromolecule base PTC material
Material and preparation method thereof.
Background technique
Ptc material is a kind of heat-sensitive semiconductive material with positive temperature coefficient, and the resistance value of material is when temperature is lower
Interior holding is basically unchanged or only small change, and when temperature is more than Curie temperature, the resistance value of material with temperature liter
Height sharply increases.PTC material is different by the matrix of material, can be divided into ceramic matrix PTC material and high molecular based PTC
Conducing composite material.Wherein high molecular based PTC material has preparation simple, and the advantages such as at low cost are widely studied at present and answer
With.
Polymer PTC material is mostly simple binary composite construction the most at present, be using high molecular polymer as matrix, it is internal
Conductive material such as graphite powder, carbon black, multi-walled carbon nanotube etc. is filled, this structure results in material and is easy in use
Existing unstable, the problems such as leakage, and the Curie temperature of material is higher, generally between 50-400 DEG C, such some disadvantages
Apply high molecular based PTC material can not well in room temperature thermal control field.Room temperature of the Cheng Wen dragon et al. in application in 2013
The patent of invention of the compound ptc material of thermal control and the article A new kind of shape- delivered in 2014
One kind is proposed in stabilized PCMs with positive temperature coefficient (PTC) effect
Novel normal-temperature high molecular based PTC material, structure are paraffin or other alkane as phase transformation matrix, and low density polyethylene (LDPE) is as branch
Timbering material, graphite powder is as conductive filler.Although room temperature Curie temperature may be implemented in this material, but since its material is in
Rigidity, can not filming the problems such as, good practical application can not be obtained.
In recent years, electronic computer industry development is rapid, and the requirement to thermal control also increases accordingly.It is used as and is added by ptc material
The Active thermal control system of thermal resistance becomes mainstream gradually.In telecommunications field high-end at present, such as 5G communication, Grace weight
The fields such as field of force satellite, thermal control problem become a major issue for hindering field development.However current developed room
Warm ptc material, which is not sufficient to be applied to, to need to carry out further the performance of room temperature ptc material in high-precision Active thermal control system
Optimization.
Summary of the invention
Technical problem to be solved by the present invention lies in: it cannot achieve flexibility for existing room temperature ptc material and can not
It realizes that material film leads to not the problem of being applied to room temperature high precision temperature control, it is flexible high to provide a kind of room temperature thermal control
Molecule matrix PTC material and preparation method thereof, while guaranteeing that material prepared has preferable flexible and can prepare material
At film-form.
The present invention solves above-mentioned technical problem using following technical scheme:
A kind of room temperature thermal control flexible macromolecule matrix PTC material, including block copolymer, phase transformation matrix and conductive filler,
Wherein the mass ratio of the block copolymer and phase transformation matrix is (20: 80)~(40: 60)；The mass ratio of the conductive filler
Example is less than 80%.
Further, the block copolymer is ethylene octene block copolymer, density 0.800-0.900g/cm3。
Further, the phase transformation matrix is paraffin or alkanes substance；Wherein the paraffin is solid paraffin；It is described
Alkanes substance is one of n-tetradecane~n-docosane.
Further, the conductive filler be graphite powder, conductive black, expanded graphite, multi-walled carbon nanotube, graphene,
Any one in silver-plated glass beads, conductive carbon fibre or mixture.
Further, the conductive filler be graphite powder, granularity >=95% of the powdered graphite (GP), partial size≤
30um；The graphite powder is 30-50% with the mass fraction in flexible macromolecule matrix PTC material in the room temperature thermal control.
Further, the conductive filler is conductive black, and the specific surface area of the conductive black (CB) is 10-
3000m2/g；The conductive black is 5- with the mass fraction in flexible macromolecule matrix PTC material in the room temperature thermal control
20%.
Further, a kind of preparation method of room temperature thermal control flexible macromolecule matrix PTC material, comprising the following steps:
(1) it under the conditions of 120-170 DEG C, by block copolymer, phase transformation matrix melting mixing under vacuum conditions, and stirs
Uniformly；
(2) conductive filler is added into the reaction mass of step (1), and under 120-170 DEG C, vacuum condition, stir
It is uniformly mixed, obtains mixture；
(3) mixture of step (2) is put into compression moulding in mold, be cooled to room temperature to get.
Further, the mixture of step (2) is put into mold to be pressed into thickness using hot press big in the step (3)
In the film ptc material of 0.1mm.
The technology of the present invention the utility model has the advantages that according to the mechanism of production of room temperature high molecular based PTC material PTC effect, in paraffin and
Block copolymer is added in the composite material of graphite powder or conductive black as backing material, and matching by adjusting each component
Side so that the Curie temperature that the material prepared generates PTC effect is -10~40 DEG C, and has preferable flexible and can be thin
The room temperature thermal control flexible PCT material of membranization.In addition, the compound ptc material of this room temperature thermal control prepare raw material sources extensively,
Preparation method simple possible, prepared ptc material have preferable ptc characteristics and flexibility, can preferably be applied to
The active temperature control of electronic device and other room temperature thermal control fields compensate for current room temperature ptc material and do not have flexibility and can not be thin
The defect of membranization.
Detailed description of the invention
Fig. 1 is the electricalresistivityρ of paraffinic base flexible PCT material described in the embodiment of the present invention 1 with temperature T change curve；
Fig. 2 a is that the embodiment of the present invention 2 is the non-pressurized state signal at room temperature of prepared octadecyl flexible PCT material
Figure；
Fig. 2 b embodiment of the present invention 2 is status diagram after prepared octadecyl flexible PCT material presses at room temperature.
Specific embodiment
For convenient for those skilled in the art understand that technical solution of the present invention, now in conjunction with Figure of description to the technology of the present invention side
Case is described further.
The source of following embodiment material therefor is described as follows:
The density of ethylene octene block copolymer (OBC) is 0.887g/cm3, by Dow, company is provided；Paraffin is solid
Body paraffin (44-46 DEG C of fusing point) is provided by Japanese Wako chemical reagents corporation；N-octadecane, n-eicosane and n-heptadecane by
Aladdin reagent Co., Ltd provides；Granularity >=95% of powdered graphite (GP), partial size≤30um are tried by Chinese medicines group chemistry
Agent Co., Ltd provides；The specific surface area of carbon black (CB) is 45m2/ g is provided by Hefei Ke Jing Materials Technology Ltd..
Embodiment 1
Steps are as follows for a kind of specific preparation manipulation of room temperature thermal control flexible macromolecule matrix PTC material:
(1) 45g ethylene octene block copolymer (OBC) and 105g paraffin are added in stainless steel autoclave body, cover sealing cover
It is tamping, then stainless steel autoclave body is put into thermostatical oil bath, vacuum pump is connected to the pumping of upper stainless steel autoclave body by rubber tube
Port, it is intracavitary to autoclave body to vacuumize, under the conditions of 150-170 DEG C of temperature, 300 revs/min of revolving speed, stirred with digital display constant speed
Machine is uniformly mixed；
(2) 100g powdered graphite (GP) is added, under 150-170 DEG C of temperature, vacuum condition, with 300 revs/min of revolving speed
Stirring, is uniformly mixed, obtains mixture；
(3) mixture is pressed into the wafer sample that diameter is 30mm thickness 5mm by hot press, it is fixed to be cooled to room temperature
Type stands 3-5 hours, to its stable structure, can obtain the paraffinic base flexible PCT material of sheet；It is applied on wafer sample two sides
Upper conductive silver glue is dry to get room temperature thermal control flexible macromolecule matrix PTC material product to conductive silver glue as electrode.
(ρ is material to each component mass ratio and its low-temperature resistivity ρ that table 1 is prepared paraffinic base flexible PCT material
Resistivity at 10 DEG C).
The each component mass ratio and its low-temperature resistivity ρ of 1 paraffinic base flexible PCT material of table
| Quality of Paraffin Waxes score | Graphite powder mass fraction | OBC mass fraction | OBC/ Quality of Paraffin Waxes ratio | Low-temperature resistivity |
| 42% | 40% | 18% | 30∶70 | 1862Ω.cm |
Within the scope of 10 DEG C to 50 DEG C, is heated with the 1.2 DEG C/min rate of heat addition to ptc material sample, measure its electricalresistivityρ
With temperature T change curve, as shown in Figure 1, ordinate takes the denary logarithm form of ρ to indicate.From figure 1 it appears that
The Curie temperature of the PTC sample meets the requirement of room temperature Curie temperature at 22 DEG C or so, it can be seen that the low-temperature resistance at 10 DEG C
Rate is 1800 Ω .cm or so, significantly less than common paraffin matrix PTC material.
Embodiment 2
Steps are as follows for a kind of specific preparation manipulation of room temperature thermal control flexible macromolecule matrix PTC material:
(1) 45g ethylene octene block copolymer (OBC) and 105g n-octadecane are added in stainless steel autoclave body, are covered close
Capping is tamping, and then stainless steel autoclave body is put into thermostatical oil bath, and vacuum pump is connected upper stainless steel autoclave body by rubber tube
Bleeding point, it is intracavitary to autoclave body to vacuumize, under the conditions of 150-170 DEG C of temperature, 300 revs/min of revolving speed, with digital display constant speed
Blender is uniformly mixed；
(2) 100g powdered graphite (GP) is added, under 150-170 DEG C of temperature, vacuum condition, with 300 revs/min of revolving speed
Stirring, is uniformly mixed, obtains mixture；
(3) mixture is pressed into the film of 140mm*70mm*0.8mm by hot press, is cooled to room temperature sizing, is stood
6-8 hours, to its stable structure, film-form octadecyl flexible PCT material can be obtained.
Three are carried out to the octadecyl flexible PCT material of formation and presses experiment, tests its flexibility, is as shown in Figure 2 a not apply
The status diagram of octadecyl flexible PCT material when pressure, Fig. 2 b are that the state of the octadecyl flexible PCT material after pressure is shown
It is intended to, can be seen that the material keeps good flexibility at room temperature by comparison.
Embodiment 3
Steps are as follows for a kind of specific preparation manipulation of room temperature thermal control flexible macromolecule matrix PTC material:
(1) 45g ethylene octene block copolymer (OBC) and 135g paraffin are added in stainless steel autoclave body, cover sealing cover
It is tamping, then stainless steel autoclave body is put into thermostatical oil bath, vacuum pump is connected to the pumping of upper stainless steel autoclave body by rubber tube
Port, it is intracavitary to autoclave body to vacuumize, under the conditions of 150-170 DEG C of temperature, 300 revs/min of revolving speed, stirred with digital display constant speed
Machine is uniformly mixed；
(2) 20g conductive black (CB) is added, under 150-170 DEG C of temperature, vacuum condition, with 300 revs/min of revolving speed
Stirring, is uniformly mixed, obtains mixture；
(3) mixture is pressed into the wafer sample that diameter is 30mm thickness 5mm by hot press, it is fixed to be cooled to room temperature
Type stands 3-5 hours, to its stable structure, can obtain the paraffinic base flexible PCT material of sheet；It is applied on wafer sample two sides
Upper conductive silver glue is dry to get room temperature thermal control flexible macromolecule matrix PTC material product to conductive silver glue as electrode.
(ρ is material to each component mass ratio and its low-temperature resistivity ρ that table 2 is prepared paraffinic base flexible PCT material
Resistivity at 10 DEG C).
The each component mass ratio and its low-temperature resistivity ρ of 2 paraffinic base flexible PCT material of table
| Quality of Paraffin Waxes score | Carbon black mass score | OBC mass fraction | OBC/ Quality of Paraffin Waxes ratio | Low-temperature resistivity |
| 67.5% | 10% | 22.5% | 25∶65 | 1143Ω.cm |
Claims (8)
1. a kind of room temperature thermal control flexible macromolecule matrix PTC material, which is characterized in that including block copolymer, phase transformation matrix and
Conductive filler, wherein the mass ratio of the block copolymer and phase transformation matrix is (20: 80)~(40: 60)；The conduction is filled out
The mass ratio of material is less than 80%.
2. a kind of room temperature thermal control flexible macromolecule matrix PTC material according to claim 1, which is characterized in that described
Block copolymer is ethylene octene block copolymer.
3. a kind of room temperature thermal control flexible macromolecule matrix PTC material according to claim 1, which is characterized in that described
Phase transformation matrix is paraffin or alkanes substance；Wherein the paraffin is solid paraffin；The alkanes substance is n-tetradecane
One of~n-docosane.
4. a kind of room temperature thermal control flexible macromolecule matrix PTC material according to claim 1, which is characterized in that described
Conductive filler is graphite powder, conductive black, expanded graphite, multi-walled carbon nanotube, graphene, silver-plated glass beads, conductive carbon fibres
Any one in dimension or mixture.
5. a kind of room temperature thermal control flexible macromolecule matrix PTC material according to claim 4, which is characterized in that described
Conductive filler is graphite powder, and the graphite powder is in the mass fraction of the room temperature thermal control in flexible macromolecule matrix PTC material
For 30-50%.
6. a kind of room temperature thermal control flexible macromolecule matrix PTC material according to claim 5, which is characterized in that described
Conductive filler is conductive black, and the conductive black is in the quality of the room temperature thermal control in flexible macromolecule matrix PTC material
Score is 5-20%.
7. a kind of method for preparing room temperature thermal control flexible macromolecule matrix PTC material as claimed in any one of claims 1 to 6,
It is characterized in that, comprising the following steps:
(1) it under the conditions of 120-170 DEG C, by block copolymer, phase transformation matrix melting mixing under vacuum conditions, and stirs equal
It is even；
(2) conductive filler is added into the reaction mass of step (1), and under 120-170 DEG C, vacuum condition, is stirred
Uniformly, mixture is obtained；
(3) mixture of step (2) is put into compression moulding in mold, be cooled to room temperature to get.
8. a kind of preparation method of room temperature thermal control flexible macromolecule matrix PTC material according to claim 7, feature exist
In the mixture of step (2) to be put into mold to be pressed into thickness using hot press thin greater than 0.1mm in the step (3)
Film ptc material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881297A (en) * | 2019-03-01 | 2019-06-14 | 苏州城邦达力材料科技有限公司 | A kind of variable composition of electric property, nanofiber and preparation method thereof |
| CN110283497A (en) * | 2019-06-28 | 2019-09-27 | 深圳烯材科技有限公司 | A method of printing the silk-screened conductive ink of accurate self limiting temperature flexible electrothermal membrane |
| CN113088030A (en) * | 2021-03-29 | 2021-07-09 | 北京科技大学 | Flexible phase-change composite material with cross-linked network structure and preparation method thereof |
| CN115141493A (en) * | 2022-06-28 | 2022-10-04 | 中国科学技术大学 | Preparation method of compressible high-flexibility high-heat-capacity phase-change heat-conducting interface material |
| CN117166163A (en) * | 2023-11-02 | 2023-12-05 | 启东市久新印染有限公司 | Auxiliary washing device for fabric processing |
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