W-Cu composite powder with high thermal conductivity and low thermal expansion coefficient and preparation method thereof

Abstract

The invention discloses W-Cu composite powder with high thermal conductivity and low thermal expansion coefficient. The thermal conductivity is 200-235W / (m.K), and the thermal expansion coefficient is (5.6-9.3) * 10<-6> / K. The invention further discloses a preparation method of the W-Cu composite powder with high thermal conductivity and low thermal expansion coefficient. The preparation method comprises the following steps of: preparing a W-Cu precursor by adopting a wet chemical method; carrying out pyrolysis reduction on the W-Cu precursor in a hydrogen environment; and carrying out compression molding on the reduced W-Cu composite powder, then heating to 1100-1300 DEG C in a hydrogen atmosphere, carrying out heat preservation for 100-140 minutes, and cooling to obtain the W-Cu composite powder. According to the preparation method, the W-Cu composite precursor is prepared by adopting the wet chemical method, the W-Cu composite powder with high sintering activity is obtained through different reduction process combinations, and then the W-Cu composite powder with high density, high thermal conductivity, low thermal expansion coefficient and uniform tissue distribution is prepared through subsequent liquid phase sintering.

Description

technical field

[0001] The invention relates to the technical field of integrated circuit packaging materials, in particular to a chemical preparation method of W-Cu composite powder with high thermal conductivity and low thermal expansion coefficient and its composite material. Background technique

[0002] In integrated circuits, electronic packaging materials play the role of chip protection, chip support, chip heat dissipation, chip insulation and chip and external circuit connection, which requires packaging materials to have excellent electrical conductivity, thermal conductivity, good chemical inertia, low thermal expansion coefficient and high hardness and so on. With the rapid development of microelectronics technology, integrated circuits are gradually becoming highly integrated and miniaturized, which means that packaging materials need to release heat in a timely manner, and have a low thermal expansion coefficient to ensure compatibility with Si, Semiconductor ...

Examples

Embodiment 1

[0027] The preparation method of high thermal conductivity, low thermal expansion coefficient W-Cu composite powder is as follows:

[0028] Step 1: Precursor Preparation

[0029] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%) and copper nitrate (Cu(NO 3 ) 2 ·3H 2 O, Aladdin, purity ≥ 99.5%) are dissolved in deionized water, heated and stirred to obtain a mixed solution, and after the mixed solution is transparent, add oxalic acid (C 2 h 2 o 4 2H 2 O, analytically pure), the precipitate obtained after the mixed solution was stirred and evaporated to dryness is the W-Cu precursor.

[0030] Among them, the addition amount of copper nitrate and oxalic acid is 70.41% and 39% of the mass of ammonium metatungstate respectively.

[0031] Step 2: Hydrogen reduction

[0032] Fully grind the massive precursor obtained in step 1 in a mortar to obtain fine powder, put the burning boat containing the fine powder into a hydrogen (hydrogen purity ≥ 99.999%) reduction furnace f...

Embodiment 2

[0040] The chemical preparation method of W-Cu composite powder with high thermal conductivity and low thermal expansion coefficient is as follows:

[0041] Step 1: Precursor preparation

[0042] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%) and copper nitrate (Cu(NO 3 ) 2 ·3H 2 O, Aladdin, purity ≥ 99.5%) are dissolved in deionized water, heated and stirred to obtain a mixed solution, and after the mixed solution is transparent, add oxalic acid (C 2 h 2 o 4 2H 2 O, analytically pure), the precipitate obtained after the mixed solution was stirred and evaporated to dryness is the W-Cu precursor.

[0043] Wherein, the addition amount of copper nitrate and oxalic acid is respectively 31.29% and 38% of the mass of ammonium metatungstate.

[0044] Step 2: Hydrogen reduction

[0045] Fully grind the massive precursor obtained in step 1 in a mortar to obtain fine powder, put the burning boat containing the fine powder into a hydrogen (hydrogen purity ≥ 99.999%) reduc...

Embodiment 3

[0050] The preparation method of high thermal conductivity, low thermal expansion coefficient W-Cu composite powder is as follows:

[0051] Step 1: Precursor preparation

[0052] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%) and copper nitrate (Cu(NO 3 ) 2 ·3H 2 O, Aladdin, purity ≥ 99.5%) are dissolved in deionized water, heated and stirred to obtain a mixed solution, and after the mixed solution is transparent, add oxalic acid (C 2 h 2 o 4 2H 2 O, analytically pure), the precipitate obtained after the mixed solution was stirred and evaporated to dryness is the W-Cu precursor.

[0053] Wherein, the addition amounts of copper nitrate and oxalic acid are respectively 120.70% and 40% of the mass of ammonium metatungstate.

[0054] Step 2: Hydrogen reduction

[0055] Fully grind the massive precursor obtained in step 1 in a mortar to obtain fine powder, put the burning boat containing the fine powder into a hydrogen (hydrogen purity ≥ 99.999%) reduction furnace f...

technical field

[0001] The invention relates to the technical field of integrated circuit packaging materials, in particular to a chemical preparation method of W-Cu composite powder with high thermal conductivity and low thermal expansion coefficient and its composite material. Background technique

[0002] In integrated circuits, electronic packaging materials play the role of chip protection, chip support, chip heat dissipation, chip insulation and chip and external circuit connection, which requires packaging materials to have excellent electrical conductivity, thermal conductivity, good chemical inertia, low thermal expansion coefficient and high hardness and so on. With the rapid development of microelectronics technology, integrated circuits are gradually becoming highly integrated and miniaturized, which means that packaging materials need to release heat in a timely manner, and have a low thermal expansion coefficient to ensure compatibility with Si, Semiconductor ...

Examples

Embodiment 1

[0027] The preparation method of high thermal conductivity, low thermal expansion coefficient W-Cu composite powder is as follows:

[0028] Step 1: Precursor Preparation

[0029] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%) and copper nitrate (Cu(NO 3 ) 2 ·3H 2 O, Aladdin, purity ≥ 99.5%) are dissolved in deionized water, heated and stirred to obtain a mixed solution, and after the mixed solution is transparent, add oxalic acid (C 2 h 2 o 4 2H 2 O, analytically pure), the precipitate obtained after the mixed solution was stirred and evaporated to dryness is the W-Cu precursor.

[0030] Among them, the addition amount of copper nitrate and oxalic acid is 70.41% and 39% of the mass of ammonium metatungstate respectively.

[0031] Step 2: Hydrogen reduction

[0032] Fully grind the massive precursor obtained in step 1 in a mortar to obtain fine powder, put the burning boat containing the fine powder into a hydrogen (hydrogen purity ≥ 99.999%) reduction furnace f...

Embodiment 2

[0040] The chemical preparation method of W-Cu composite powder with high thermal conductivity and low thermal expansion coefficient is as follows:

[0041] Step 1: Precursor preparation

[0042] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%) and copper nitrate (Cu(NO 3 ) 2 ·3H 2 O, Aladdin, purity ≥ 99.5%) are dissolved in deionized water, heated and stirred to obtain a mixed solution, and after the mixed solution is transparent, add oxalic acid (C 2 h 2 o 4 2H 2 O, analytically pure), the precipitate obtained after the mixed solution was stirred and evaporated to dryness is the W-Cu precursor.

[0043] Wherein, the addition amount of copper nitrate and oxalic acid is respectively 31.29% and 38% of the mass of ammonium metatungstate.

[0044] Step 2: Hydrogen reduction

[0045] Fully grind the massive precursor obtained in step 1 in a mortar to obtain fine powder, put the burning boat containing the fine powder into a hydrogen (hydrogen purity ≥ 99.999%) reduc...

Embodiment 3

[0050] The preparation method of high thermal conductivity, low thermal expansion coefficient W-Cu composite powder is as follows:

[0051] Step 1: Precursor preparation

[0052] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%) and copper nitrate (Cu(NO 3 ) 2 ·3H 2 O, Aladdin, purity ≥ 99.5%) are dissolved in deionized water, heated and stirred to obtain a mixed solution, and after the mixed solution is transparent, add oxalic acid (C 2 h 2 o 4 2H 2 O, analytically pure), the precipitate obtained after the mixed solution was stirred and evaporated to dryness is the W-Cu precursor.

[0053] Wherein, the addition amounts of copper nitrate and oxalic acid are respectively 120.70% and 40% of the mass of ammonium metatungstate.

[0054] Step 2: Hydrogen reduction

[0055] Fully grind the massive precursor obtained in step 1 in a mortar to obtain fine powder, put the burning boat containing the fine powder into a hydrogen (hydrogen purity ≥ 99.999%) reduction furnace f...

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