阅读说明：本技术 一种多晶硅铸锭炉用碳纤维石墨材料及其制备方法 (A kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material and preparation method thereof ) 是由 闵洁 张培林 庞中海 武建军 刘伟凯 纪永良 雷涛 霍有 张彦举 于 2019-09-02 设计创作，主要内容包括：本发明涉及石墨材料的技术领域,特别是涉及一种多晶硅铸锭炉用碳纤维石墨材料及其制备方法,其原料选择合理,各项理化性能优越,制备工艺科学；包括混合料和粘结剂,所述混合料与粘结剂的重量比为70:30~72:28所述混合料由骨料和粉料组成,所述骨料、粉料的重量比为65:35~70:30,所述骨料为针状石油焦,所述粉料为碳纤维、沥青焦和炭黑,所述碳纤维、沥青焦和炭黑的重量比为35:40:25,所述粘结剂为改质中温煤沥青；其制备方法包括以下步骤：(1)粉碎配料；(2)混捏；(3)振动成型；(4)一次焙烧；(5)浸渍；(6)二次隧道窑焙烧；(7)石墨化；(8)机加工。(The present invention relates to the technical fields of graphite material, and more particularly to a kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material and preparation method thereof, rationally, every physicochemical property is superior for raw material selection, preparation process science；Including mixture and binder, the weight ratio of the mixture and binder is that mixture described in 70:30 ~ 72:28 is made of aggregate and powder, the aggregate, powder weight ratio be 65:35 ~ 70:30, the aggregate is acicular petroleum coke, the powder is carbon fiber, pitch coke and carbon black, the weight ratio of the carbon fiber, pitch coke and carbon black is 35:40:25, and the binder is modification medium temperature coal pitch；Preparation method includes the following steps: (1) crushing ingredient；(2) kneading；(3) vibration moulding；(4) primary roasting；(5) it impregnates；(6) secondary tunnel oven roasting；(7) it is graphitized；(8) it machines.)

1. a kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material, which is characterized in that including mixture and binder, the mixing The weight ratio of material and binder is 70:30 ~ 72:28, and the mixture is made of aggregate and powder, the weight of the aggregate and powder Amount is than being 65:35 ~ 70:30, and the aggregate is acicular petroleum coke, and the powder is carbon fiber, pitch coke and carbon black, the carbon fiber The weight ratio of dimension, pitch coke and carbon black is 35:40:25, and the binder is modification medium temperature coal pitch.

2. a kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material as described in claim 1, which is characterized in that percentage by weight Content meter, the acicular petroleum coke broken particle size range and content are as follows:

1 μm of 15 ~ 25wt% of partial size≤0.5 μm <；

0.5 μm of 20 ~ 25wt% of partial size≤0.3 μm <；

0.3 μm of 15 ~ 25wt% of partial size≤0.1 μm <；

0 0.1 μm of 45 ~ 50wt% of m of < partial size <.

3. a kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material as claimed in claim 2, which is characterized in that percentage by weight Content meter, the broken particle size range of the acicular petroleum coke and content are preferred are as follows:

1 μm of partial size≤0.5 μm < 20wt%；

0.5 μm of partial size≤0.3 μm < 25wt%；

0.3 μm of partial size≤0.1 μm < 20wt%；

0 0.1 μm of 45wt% of < partial size <.

4. a kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material as claimed in claim 3, which is characterized in that The following steps are included:

(1) it crushes ingredient: carrying out ingredient after aggregate and powder are crushed and screened in proportion；

(2) kneading: the ingredient through being classified is added in kneading pot and is stirred；

(3) vibration moulding: the product of kneading is subjected to vibration moulding by vibrating forming machine after kneading, passes through hydraulic pressurization By thickener jolt ramming, demoulding is placed in water to be cooled to room temperature swing die, and the bulk density of green compact after molding reaches 1.80 ~ 2.1g/cm³, briquetting pressure >=10MPa, the dwell time >=5min；

(4) primary roasting: green compact after molding being put into carbonizing apparatus, are filled in furnace using coke powder, quartz sand, river sand etc., It in the case where completely cutting off air, is gradually heated by heating curve, carries out carbonization heating and fire；

(5) it impregnates: the product after roasting being preheating to 350 ~ 450 DEG C, retention time 8h, then the product after roasting is placed in dipping It in tank, will be vacuumized in impregnating autoclave, pressurize 2.5h, impregnating agent is injected in impregnating autoclave, pressure maintaining 2h, so that impregnating agent is immersed roasting and produces In sample wells gap；

(6) secondary tunnel oven roasting: the product process of passing through tunnel kiln after dipping is subjected to Fast Sintering pitch, maximum temperature is 700 DEG C, calcining time 144h；

(7) it is graphitized: the product after after baking being put into acheson furnace, in the absence of air conditions, is passed through Roasting product is heated to 2800 ~ 3200 DEG C by electric current, so that two-dimensional structure carbon product is converted to three-dimensional graphite network, when power transmission is total Between 168h；

(8) it machines: being machined out processing to by graphited product.

5. a kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material as claimed in claim 4, which is characterized in that Kneading in the step (2) is divided into dry-mixed and wet mixing, it is described it is dry-mixed be that aggregate and powder are added in kneading pot and are stirred, Kneading pot is double reamer types, and kneading pot temperature is 220 ~ 250 DEG C, and the dry-mixed temperature of aggregate powder is 150 ~ 180 DEG C, and the dry-mixed time is 45~50min；Wet mixing binder temperature is 140 ~ 180 DEG C, and the wet mixing time is 40 ~ 45min.

6. a kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material as claimed in claim 4, which is characterized in that Heating curve in the step (4) are as follows: at 150 ~ 350 DEG C, heating rate is 3.0 ~ 4.0 DEG C/h, retention time 55h；In At 350 ~ 450 DEG C, heating rate is 1.5 ~ 1.8 DEG C/h, retention time 35h；At 450 ~ 550 DEG C, heating rate is 1.2 ~ 1.4 DEG C/h, retention time 85h；At 550 ~ 650 DEG C, heating rate is 1.8 ~ 2.0 DEG C/h, retention time 55h；At 650 ~ 750 DEG C When, heating rate is 3.5 ~ 4.0 DEG C/h, and the retention time is for 24 hours；At 750 ~ 850 DEG C, heating rate is 4.0 ~ 5.0 DEG C/h, is kept Time is for 24 hours；At 850 ~ 1150 DEG C, heating rate is 6.5 ~ 8.5 DEG C/h, retention time 30h；At 1150 ~ 1250 DEG C, heating Rate is 8.0 ~ 8.5 DEG C/h, and the retention time is for 24 hours；22h is kept at 1250 DEG C, then cooled to room temperature is come out of the stove.

7. a kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material as claimed in claim 4, which is characterized in that Impregnating agent used in the step (5) is impregnating pitch.

8. a kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material as claimed in claim 4, which is characterized in that Specific heating procedure in the step (7) is with the heating rate of 250 DEG C/h, from room temperature to 1350 DEG C, then with 25 DEG C/heating rate of h is warming up to 2200 DEG C from 1350 DEG C, 3200 DEG C are freely warming up to after temperature reaches 2200 DEG C.

Technical field

The present invention relates to the technical fields of graphite material, more particularly to a kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material Material and preparation method thereof.

Background technique

Graphite have good thermal conductance and heat-resisting quantity, during applied at elevated temperature, thermal expansion coefficient is small, to it is anxious heat, Chilling has certain stain resistance energy.To acid, the corrosion resistance of alkaline solution is stronger, has excellent chemical stability.

There are many places in semiconductor, solar energy power generating field silicon wafer growth apparatus graphite member, such as graphite crucible, stone Adopt graphite seat, graphite insulation cover and graphite thermal insulation material etc. outside black thermal field, graphite cover board, silicon wafer, graphite member used also with The development of silicon wafer size technologies, it is desirable that the materials such as graphite crucible, graphite field high-purity, enlargement, and to the sharp skill of high-endization essence Art development.

Summary of the invention

In order to solve the above technical problems, the purpose of the present invention is to provide a kind of selection of raw material is reasonable, every physicochemical property Superior polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material；

Another object of the present invention is to provide a kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of preparation process science Preparation method.

A kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of the invention, including mixture and binder, the mixing The weight ratio of material and binder is 70:30 ~ 72:28, and the mixture is made of aggregate and powder, the weight of the aggregate and powder Amount is than being 65:35 ~ 70:30, and the aggregate is acicular petroleum coke, and the powder is carbon fiber, pitch coke and carbon black, the carbon fiber The weight ratio of dimension, pitch coke and carbon black is 35:40:25, and the binder is modification medium temperature coal pitch.

Real density >=2.15g/cm of the aggregate acicular petroleum coke³, ash content≤0.25%, volatile matter≤0.30%, sulphur contains Amount≤0.50%；

The granularity of the powder carbon fiber is 0.3 ~ 0.7 μm, tensile strength 7.0Gpa, density 2.12g/cm³, resistivity≤30 μ Ωcm；

The granularity of the powder pitch coke is 0.5 ~ 1.0 μm, real density >=2.13/cm³, ash content≤0.25%, sulfur content≤ 0.3%, fugitive constituent≤0.3%；

The purity 99% of the powder carbon black, partial size are 0.4 ~ 0.8 μm；

The softening point of the binder modification medium temperature coal pitch is 83 ~ 86 DEG C, and coking value is >=48%, ash content≤0.30%；

A kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of the invention, weight percentage, the acicular petroleum coke Broken particle size range and content are as follows:

1 μm of 15 ~ 25wt% of partial size≤0.5 μm <；

0.5 μm of 20 ~ 25wt% of partial size≤0.3 μm <；

0.3 μm of 15 ~ 25wt% of partial size≤0.1 μm <；

0 0.1 μm of 45 ~ 50wt% of m of < partial size <.

A kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of the invention, weight percentage, the needle-shaped stone The broken particle size range of oil coke and content are preferred are as follows:

1 μm of partial size≤0.5 μm < 20wt%；

0.5 μm of partial size≤0.3 μm < 25wt%；

0.3 μm of partial size≤0.1 μm < 20wt%；

0 0.1 μm of 45wt% of < partial size <.

A kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of the invention, comprising the following steps:

(1) it crushes ingredient: carrying out ingredient after aggregate and powder are crushed and screened in proportion；

(2) kneading: the ingredient through being classified is added in kneading pot and is stirred；

(3) vibration moulding: the product of kneading is subjected to vibration moulding by vibrating forming machine after kneading, passes through hydraulic pressurization By thickener jolt ramming, demoulding is placed in water to be cooled to room temperature swing die, and the bulk density of green compact after molding reaches 1.80 ~ 2.1g/cm³, briquetting pressure >=10MPa, the dwell time >=5min；

(4) primary roasting: green compact after molding being put into carbonizing apparatus, are filled in furnace using coke powder, quartz sand, river sand etc., It in the case where completely cutting off air, is gradually heated by heating curve, carries out carbonization heating and fire；

(5) it impregnates: the product after roasting being preheating to 350 ~ 450 DEG C, retention time 8h, then the product after roasting is placed in dipping It in tank, will be vacuumized in impregnating autoclave, pressurize 2.5h, impregnating agent is injected in impregnating autoclave, pressure maintaining 2h, so that impregnating agent is immersed roasting and produces In sample wells gap；

(6) secondary tunnel oven roasting: the product process of passing through tunnel kiln after dipping is subjected to Fast Sintering pitch, maximum temperature is 700 DEG C, calcining time 144h；

(7) it is graphitized: the product after after baking being put into acheson furnace, in the absence of air conditions, is passed through Roasting product is heated to 2800 ~ 3200 DEG C by electric current, so that two-dimensional structure carbon product is converted to three-dimensional graphite network, when power transmission is total Between 168h；

(8) it machines: being machined out processing to by graphited product.

A kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of the invention, it is mixed in the step (2) Pinch and be divided into dry-mixed and wet mixing, it is described it is dry-mixed be that aggregate and powder are added in kneading pot to be stirred, kneading pot is double reamer types, Kneading pot temperature is 220 ~ 250 DEG C, and the dry-mixed temperature of aggregate powder is 150 ~ 180 DEG C, and the dry-mixed time is 45 ~ 50min；Wet mixing bonding Agent temperature is 140 ~ 180 DEG C, and the wet mixing time is 40 ~ 45min.

A kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of the invention, the liter in the step (4) Warm curve are as follows: at 150 ~ 350 DEG C, heating rate is 3.0 ~ 4.0 DEG C/h, retention time 55h；At 350 ~ 450 DEG C, heating speed Rate is 1.5 ~ 1.8 DEG C/h, retention time 35h；At 450 ~ 550 DEG C, heating rate is 1.2 ~ 1.4 DEG C/h, retention time 85h； At 550 ~ 650 DEG C, heating rate is 1.8 ~ 2.0 DEG C/h, retention time 55h；At 650 ~ 750 DEG C, heating rate be 3.5 ~ 4.0 DEG C/h, the retention time is for 24 hours；At 750 ~ 850 DEG C, heating rate is 4.0 ~ 5.0 DEG C/h, and the retention time is for 24 hours；850 ~ At 1150 DEG C, heating rate is 6.5 ~ 8.5 DEG C/h, retention time 30h；At 1150 ~ 1250 DEG C, heating rate is 8.0 ~ 8.5 DEG C/h, the retention time is for 24 hours；22h is kept at 1250 DEG C, then cooled to room temperature is come out of the stove.

A kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of the invention, the step (5) is middle to be made Impregnating agent is impregnating pitch.

The softening point of impregnating pitch is 83 ~ 88 DEG C, and coking value is >=48%, quinoline insolubles≤0.30%.

A kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material of the invention, the tool in the step (7) Body heating procedure be with the heating rate of 250 DEG C/h, from room temperature to 1350 DEG C, then with the heating rate of 25 DEG C/h from 1350 DEG C are warming up to 2200 DEG C, are freely warming up to 3200 DEG C after temperature reaches 2200 DEG C.

Compared with prior art the invention has the benefit that the purpose of the present invention is to existing graphite material manufacturing process Substantial improvements are carried out, provide a kind of selection of raw material rationally, preparation process science etc. is produced respectively with the method and material The good high-purity of physicochemical property, macrofossil ink material, will test the obtained graphite material of the present invention, and bulk density >= 1.85g/cm³, resistivity≤8.0 μ Ω m, flexural strength >=35Mpa, compression strength >=65Mpa, purity >=99.99%.

Specific embodiment

With reference to embodiment, the embodiment of the present invention is furthur described in detail.Following embodiment is used for Illustrate the present invention, but is not intended to limit the scope of the invention.