CN102332565A - Synthesis method for lithium iron phosphate/carbon composite material - Google Patents

Synthesis method for lithium iron phosphate/carbon composite material Download PDF

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CN102332565A
CN102332565A CN201110296165A CN201110296165A CN102332565A CN 102332565 A CN102332565 A CN 102332565A CN 201110296165 A CN201110296165 A CN 201110296165A CN 201110296165 A CN201110296165 A CN 201110296165A CN 102332565 A CN102332565 A CN 102332565A
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lithium
phosphate
iron phosphate
synthetic method
ball milling
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CN102332565B (en
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王连邦
施梅勤
徐土根
吴晓潭
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Zhejiang University of Technology ZJUT
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Abstract

The invention discloses a synthesis method for a lithium iron phosphate/carbon composite material. The synthesis method is characterized by comprising the following steps of: (1) uniformly mixing lithium phosphate, iron powder, iron phosphate, another lithium source and a carbonous conductive agent precursor, wherein the another lithium source is one or the combination of any of the following components: lithium carbonate, lithium oxalate, lithium acetate, lithium hydroxide and lithium nitrate, and the carbonous conductive agent precursor is one or the combination of any of the following components: glucose, sucrose, citric acid, starch, polyvinyl alcohol, stearic acid and lauric acid; (2) putting the raw material mixture obtained in the step (1) into a ball-milling container and performing full ball milling; and (3) putting the mixture subjected to the ball milling into nitrogen gas and baking the mixture at 600-800 DEG C to prepare the lithium iron phosphate/carbon composite material. The synthesis method is simple in process, and the synthesized lithium iron phosphate/carbon composite material is high in specific capacity and excellent in high-current and cycle performance.

Description

A kind of synthetic method of lithium iron phosphate
Technical field:
The present invention relates to a kind of synthetic method of lithium iron phosphate, this composite material can be used as anode material for lithium-ion batteries and uses.
Background technology:
Since LiFePO4 that people such as A.K.Padhi in 1997 report has an olivine-type structure can be used as anode material for lithium-ion batteries, owing to its excellent electrochemical properties, abundant raw material sources, good safety performance, characteristics such as can under hot environment, use to receive the favor of vast scientific research institution and commercial company.
At present, method preparing phosphate iron lithium mainly contains high temperature solid-state method, microwave process for synthesizing, sol-gel process, liquid phase deposition etc.High temperature solid-state method technology is simple, is fit to large-scale production, but the common mixing of reactant is inhomogeneous; The synthetic material particle is bigger, and divalence source of iron cost is higher, in the preparation process, occurs shortcomings such as ferric iron impurity easily; Cause material property poor, batch homogeneity of material can not get guaranteeing; Microwave process for synthesizing also is a kind of solid phase method synthetic method, and it has the reaction time short (3-10min), and energy consumption is low, and combined coefficient is high, advantages such as uniform particles, but this method requires comparatively strictness and input cost too high to process conditions, is not suitable for carrying out large-scale production; The advantage of sol-gal process is that its precursor solution chemical uniformity is good, the gel heat treatment temperature is low, the powder granule particle diameter is little and narrowly distributing, the powder sintering performance is good, course of reaction is easy to control, equipment is simple, but that gel drying shrinks is big, synthesis cycle is long, the suitability for industrialized production difficulty is bigger; The electrochemical performances of lithium iron phosphate that the liquid phase co-electrodeposition method prepares is better, but whole process all carries out under nitrogen protection atmosphere, and complex process is unfavorable for industrialization.
In high temperature sintering and charging and discharging lithium battery process, usually have the loss of part lithium salts, mainly comprise following three aspects: in high-temperature sintering process, part lithium salts decomposes causes it with Li (1) 2The form of O and volatilizing; (2) when charging and discharging lithium battery, lithium and electrolyte react and form SEI, have consumed the part lithium; (3) positive electrode in charge and discharge process along with lithium take off that the embedding meeting is corresponding to be shown as the increase of volume and reduce, repeatedly after the circulation, can cause part-structure generation deformation, the lithium ion of dissolving passes barrier film and arrives negative pole, sticks on the negative pole.Therefore, in traditional preparation process, can add excessive phosphoric acid lithium salts usually, to remedy the influence that the lithium salts loss is caused in the said process.But, can cause the not enough LiFePO4 electron mobility of congenital conductivity lower if add the excess phosphoric acid lithium because lithium phosphate is a kind of non-conductor of electricity.
Summary of the invention:
The technical problem that the present invention will solve provides a kind of synthetic method of lithium iron phosphate, and this synthetic method craft is simple, and the lithium iron phosphate specific capacity of being synthesized is high, and big electric current and cycle performance are good.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of synthetic method of lithium iron phosphate comprises the steps:
(1) lithium phosphate, iron powder, ferric phosphate, other a kind of lithium source and carbon containing conductive agent presoma are mixed; Described another one lithium source is selected from following a kind of or any several kinds combination: lithium carbonate, lithium oxalate, lithium acetate, lithium hydroxide, lithium nitrate, and the described carbonaceous conductive presoma that contains is selected from following a kind of or any several kinds combination: glucose, sucrose, citric acid, starch, polyvinyl alcohol, stearic acid, laurate; The molar ratio of described lithium phosphate, iron powder, ferric phosphate is 1: 1: 2.06; Said other a kind of lithium source is according to making that the mol ratio of lithium in the final raw mix, iron, phosphorus, oxygen is 1.02～2: add at 1.02: 1.02: 4.08, described carbon containing conductive agent presoma is 2～25wt.% of theoretical LiFePO4 quality;
(2) place ball mill container to carry out abundant ball milling step (1) gained raw mix;
(3) place nitrogen in 600～800 ℃ of roastings in the mixture behind the ball milling, can make described lithium iron phosphate.
The used raw material of the present invention as can lithium phosphate, ferric phosphate and another kind of lithium source can contain the crystallization water, for example lithium phosphate uses Li 3PO 40.5H 2O, ferric phosphate uses FePO 44H 2O, described in addition iron powder uses reduced iron powder, can reduce cost like this.
Further, in the step (1), also can add the corresponding compound of doped chemical in the raw mix; The for example oxide of doped chemical, nitrate; Oxalates, carbonate, hydroxide etc.; Described doped chemical can be selected from following a kind of or multiple combination arbitrarily: fluorine, chlorine, bromine, iodine, sulphur, nickel, cobalt, manganese, copper, zinc, titanium, silver, magnesium, zirconium, vanadium, molybdenum, aluminium, chromium, rare earth element, preferred doped chemical is: fluorine, chlorine, nickel, cobalt, copper, silver, rare earth element.Those skilled in the art can select the corresponding compound of suitable doped chemical as required from prior art.
Further, the addition of the corresponding compound of described doped chemical is 0～1: 1.02 in the ratio of the molal quantity of doped chemical and the molal quantity of theoretical LiFePO4.
Further, in the step (1), described carbon containing conductive agent presoma is preferably 3～12wt.% of theoretical LiFePO4 quality.
Further, the ball milling time in the step (2) is 1～20 hour, is preferably 2～10 hours.
Further, the roasting time in the step (3) is 1～20 hour, is preferably 4～12 hours.
The lithium iron phosphate that the present invention makes can be used as anode material for lithium-ion batteries and uses.
Compared with prior art, the method for synthesizing lithium ionic cell positive pole material lithium iron phosphate of the present invention has following outstanding feature:
(1) one or more combinations in use lithium carbonate, lithium oxalate, lithium acetate, lithium hydroxide, the lithium nitrate are as the lithium source that excessive part lithium is provided; The loss of lithium salts in sintering and the charge and discharge process can be compensated like this, nonconducting lithium phosphate can be effectively avoided existing in the synthetic product again.
(2) positive electrode of the present invention's preparation, the LiFePO4 good crystallinity, chemical property good (high, big electric current of specific capacity and cycle performance are good), material composition and proportioning are controlled easily, good stability between batch.
(3) the present invention adopts mechanical ball milling-high temperature solid-state method synthesis technique, technology simple possible.
(4) the present invention adopts relatively inexpensive reduced iron powder and four water ferric phosphates as source of iron, and is with low cost.
Description of drawings:
Fig. 1 presses the prepared LiFePO of embodiment 1 4The x-ray diffraction pattern of/C composite material;
Fig. 2 presses the prepared LiFePO of embodiment 1 4The stereoscan photograph of/C composite material;
Fig. 3 presses the prepared LiFePO of embodiment 1 4/ C composite material is anodal, and the lithium sheet is the cycle characteristics curve chart of the lithium ion battery that assembles of negative pole.
Embodiment:
With specific embodiment technical scheme of the present invention is further specified below, but protection scope of the present invention is not limited thereto:
Embodiment 1:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.2g lithium carbonate, the 2.7g citric acid mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
LiFePO4/carbon to making has been done X-ray diffraction, can be known by Fig. 1, and prepared LiFePO4 is the pure phase structure of olivine-type rhombic system, does not have the peak of other impurity in the spectrogram.Fig. 2 is LiFePO 4/ C powder amplifies 10000 times stereoscan photograph, and visible by figure, the product particle size is about 1 micron.
With active material LiFePO 4/ C powder, acetylene black, Kynoar take by weighing 0.5g altogether and are dissolved in an amount of 1-methyl-2 pyrrolidones with 8: 1: 1 ratio of mass ratio, mix the back pulp and are applied on the aluminium foil vacuum drying and process positive plate.The electrode slice of oven dry is beaten behind the sheet accurately its quality of weighing, as anode.Be to electrode with the lithium sheet simultaneously, the micropore shaped polyethylene is a barrier film, 1.0mol/L LiPF 6+ DMC is an electrolyte, in being full of the System One glove box of argon gas, is assembled into 2032 button cells with tablet press machine.
In 2.5V～4.2V voltage range, battery is carried out the constant current charge-discharge loop test.Fig. 3 is with 1C (170mAg -1) the multiplying power charging, 1C (170mAg -1) and 10C (1700mAg -1) the cycle performance of battery figure of multiplying power discharging, can know that by Fig. 3 the material of the present invention's preparation has stable cycle performance, the advantage that specific capacity is high under big electric current.
Embodiment 2:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.17g lithium carbonate, the 2.7g citric acid mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 3:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.27g lithium carbonate, the 2.7g citric acid mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 4:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.51g lithium oxalate, the 2.7g citric acid mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 5:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.57g lithium acetate, the 2.7g citric acid mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 6:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.33g lithium hydroxide, the 2.7g citric acid mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 7:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.29g lithium nitrate, the 2.7g citric acid mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 8:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.29g lithium carbonate, 2.4g sucrose mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 9:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.29g lithium carbonate, the 1.8g stearic acid mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 10:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.29g lithium carbonate, 3.1g starch mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make evengranular LiFePO 4/ C powder.
Embodiment 11:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, 0.2g lithium carbonate, 2.7g citric acid, 0.2gCo (NO 3) 2Mix.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make the even LiFePO that is doped with cobalt element 4/ C powder.
Embodiment 12:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, 0.2g lithium carbonate, 2.7g citric acid, 0.21gCeO 2Mix.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make the even LiFePO that is doped with Ce elements 4/ C powder.
Embodiment 13:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, 0.2g lithium carbonate, 2.7g citric acid, 0.22gNH 4F mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make the even LiFePO that is doped with fluorine element 4/ C powder.
Embodiment 14:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.2g lithium carbonate, the 2.7g citric acid, the 0.34g nickel phosphate mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make the even LiFePO that is doped with nickel element 4/ C powder.
Embodiment 15:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.2g lithium carbonate, the 2.7g citric acid, 0.17gCuO mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make the even LiFePO that is doped with copper 4/ C powder.
Embodiment 16:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, the 0.2g lithium carbonate, the 2.7g citric acid, 0.15gAgO mixes.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make the even LiFePO that is doped with silver element 4/ C powder.
Embodiment 17:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33gFePO 44H 2O, 0.2g lithium carbonate, 2.7g citric acid, 0.38gLa 2O 3Mix.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make the even LiFePO that is doped with lanthanum element 4/ C powder.
Embodiment 18:
Take by weighing 3.48gLi 3PO 40.5H 2O, 1.68g reduced iron powder, 9.33fFePO 44H 2O, 0.2g lithium carbonate, 2.7g citric acid, 0.23gTiO 2Mix.Put it in the ball mill container ball milling 3 hours, and placed 750 ℃ of high-temperature roastings of nitrogen 15 hours then, can make the even LiFePO that is doped with titanium elements 4/ C powder.
The LiFePO that the foregoing description 2-18 makes 4/ C powder obtains lithium ion battery according to the method assembling of embodiment 1, carries out electrochemical property test according to conventional method, and the result sees table 1, table 2, table 3 and table 4:
Table 1
Figure BDA0000094618750000081
Table 2
Figure BDA0000094618750000082
Table 3
Figure BDA0000094618750000091
Table 4
Figure BDA0000094618750000092

Claims (9)

1. the synthetic method of a lithium iron phosphate, it is characterized in that: said synthetic method comprises the steps:
(1) lithium phosphate, iron powder, ferric phosphate, other a kind of lithium source and carbon containing conductive agent presoma are mixed; Described another one lithium source is selected from following a kind of or any several kinds combination: lithium carbonate, lithium oxalate, lithium acetate, lithium hydroxide, lithium nitrate, and the described carbonaceous conductive presoma that contains is selected from following a kind of or any several kinds combination: glucose, sucrose, citric acid, starch, polyvinyl alcohol, stearic acid, laurate; The molar ratio of described lithium phosphate, iron powder, ferric phosphate is 1: 1: 2.06; Said other a kind of lithium source is according to making that the mol ratio of lithium in the final raw mix, iron, phosphorus, oxygen is 1.02～2: add at 1.02: 1.02: 4.08, described carbon containing conductive agent presoma is 2～25wt.% of theoretical LiFePO4 quality;
(2) place ball mill container to carry out abundant ball milling step (1) gained raw mix;
(3) place nitrogen in 600～800 ℃ of roastings in the mixture behind the ball milling, can make described lithium iron phosphate.
2. the synthetic method of lithium iron phosphate according to claim 1 is characterized in that: described lithium phosphate use Li 3PO 40.5H 2O, described iron powder uses reduced iron powder, and described ferric phosphate uses FePO 44H 2O.
3. the synthetic method of lithium iron phosphate according to claim 1; It is characterized in that: also add the corresponding compound of doped chemical in the described raw mix, described doped chemical can be selected from following a kind of or multiple combination arbitrarily: fluorine, chlorine, bromine, iodine, sulphur, nickel, cobalt, manganese, copper, zinc, titanium, silver, magnesium, zirconium, vanadium, molybdenum, aluminium, chromium, rare earth element.
4. the synthetic method of lithium iron phosphate according to claim 3 is characterized in that: the addition of the compound that described doped chemical is corresponding is 0～1: 1.02 in the ratio of the molal quantity of doped chemical and the molal quantity of theoretical LiFePO4.
5. according to the synthetic method of the described lithium iron phosphate of one of claim 1～3, it is characterized in that: described carbon containing conductive agent presoma is 3～12wt.% of theoretical LiFePO4 quality.
6. according to the synthetic method of the described lithium iron phosphate of one of claim 1～3, it is characterized in that: the ball milling time in the step (2) is 1～20 hour.
7. the synthetic method of lithium iron phosphate according to claim 6, it is characterized in that: the ball milling time in the step (2) is 2～10 hours.
8. according to the synthetic method of the described lithium iron phosphate of one of claim 1～3, it is characterized in that: the roasting time in the step (3) is 1～20 hour.
9. the synthetic method of lithium iron phosphate according to claim 8, it is characterized in that: the roasting time in the step (3) is 4～12 hours.
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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN102916183A (en) * 2012-10-16 2013-02-06 上海锦众信息科技有限公司 Preparation method of lithium iron phosphate composite material of lithium ion battery
CN104466118A (en) * 2014-12-27 2015-03-25 桂林理工大学 Method for synthesizing high-performance lithium iron phosphate positive material through composite doping combined in-situ polymerization
CN106602027A (en) * 2016-12-30 2017-04-26 深圳市沃特玛电池有限公司 Modified positive electrode material for lithium iron phosphate battery and preparation method of modified positive electrode material and lithium-ion battery
CN108054373A (en) * 2017-12-24 2018-05-18 扬州工业职业技术学院 A kind of new iron lithium phosphate/carbon composite and its application in lithium battery
CN108682853A (en) * 2018-04-24 2018-10-19 江西省金锂科技股份有限公司 The preparation method of LiFePO4 and by its lithium iron phosphate positive material obtained
CN109081322A (en) * 2018-11-12 2018-12-25 渤海大学 A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore
CN110620278A (en) * 2019-09-25 2019-12-27 深圳清华大学研究院 Method for recovering anode material of waste lithium iron phosphate battery
CN111261969A (en) * 2020-02-05 2020-06-09 中国科学院化学研究所 Method for recycling and regenerating lithium iron phosphate waste battery anode material
CN112573500A (en) * 2020-12-24 2021-03-30 浙江工业大学 Preparation method of vanadium-doped lithium iron phosphate-carbon composite material taking iron powder as raw material

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CN101857215A (en) * 2010-06-22 2010-10-13 中国人民解放军国防科学技术大学 Preparation method of high tap density lithium iron phosphate (LiFePO4)
CN101948101A (en) * 2010-09-09 2011-01-19 浙江瑞邦科技有限公司 Method for preparing anode material lithium iron phosphate material of lithium battery

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CN1581537A (en) * 2004-05-20 2005-02-16 上海交通大学 Method for preparing lithiumion cell positive material Iron-lithium phosphate
CN101857215A (en) * 2010-06-22 2010-10-13 中国人民解放军国防科学技术大学 Preparation method of high tap density lithium iron phosphate (LiFePO4)
CN101948101A (en) * 2010-09-09 2011-01-19 浙江瑞邦科技有限公司 Method for preparing anode material lithium iron phosphate material of lithium battery

Cited By (11)

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Publication number Priority date Publication date Assignee Title
CN102916183A (en) * 2012-10-16 2013-02-06 上海锦众信息科技有限公司 Preparation method of lithium iron phosphate composite material of lithium ion battery
CN104466118A (en) * 2014-12-27 2015-03-25 桂林理工大学 Method for synthesizing high-performance lithium iron phosphate positive material through composite doping combined in-situ polymerization
CN106602027A (en) * 2016-12-30 2017-04-26 深圳市沃特玛电池有限公司 Modified positive electrode material for lithium iron phosphate battery and preparation method of modified positive electrode material and lithium-ion battery
CN108054373A (en) * 2017-12-24 2018-05-18 扬州工业职业技术学院 A kind of new iron lithium phosphate/carbon composite and its application in lithium battery
CN108054373B (en) * 2017-12-24 2020-06-26 扬州工业职业技术学院 Lithium iron phosphate/carbon composite material and application thereof in lithium battery
CN108682853A (en) * 2018-04-24 2018-10-19 江西省金锂科技股份有限公司 The preparation method of LiFePO4 and by its lithium iron phosphate positive material obtained
CN109081322A (en) * 2018-11-12 2018-12-25 渤海大学 A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore
CN110620278A (en) * 2019-09-25 2019-12-27 深圳清华大学研究院 Method for recovering anode material of waste lithium iron phosphate battery
CN110620278B (en) * 2019-09-25 2021-07-02 深圳清华大学研究院 Method for recovering anode material of waste lithium iron phosphate battery
CN111261969A (en) * 2020-02-05 2020-06-09 中国科学院化学研究所 Method for recycling and regenerating lithium iron phosphate waste battery anode material
CN112573500A (en) * 2020-12-24 2021-03-30 浙江工业大学 Preparation method of vanadium-doped lithium iron phosphate-carbon composite material taking iron powder as raw material

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